Accessible silanol sites - beneficial for the RP-HPLC separation of constitutional and diastereomeric azaspirovesamicol isomers.

PubMed

Wenzel, Barbara; Fischer, Steffen; Brust, Peter; Steinbach, Jörg

2010-12-10

Different RP-HPLC columns (phenyl, conventional ODS, cross-linked C(18) and special end-capped C(8) and C(18) phases) were used to investigate the separation of four basic ionizable isomers. Using ACN/20mM NH(4)OAc aq., a separation was observed exclusively on RP columns with higher silanol activity at unusual high ACN concentration, indicating cation-exchange as main retention mechanism. Using MeOH/20mM NH(4)OAc aq., another separation at low MeOH concentrations was observed on both, RP columns with higher as well as RP columns with lower silanol activity, which is mainly based on hydrophobic interactions. The isomers were also separated on a bare silica column at higher MeOH content using NH(4)OAc. Since cation-exchange governs this retention, the elution order was different compared to the RP phases. A strong retention on the silica column was observed in ACN, which could be attributed to partition processes as additional retention mechanism. Copyright © 2010 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.

Chromatographic hydrogen isotope separation

DOEpatents

Aldridge, F.T.

Intermetallic compounds with the CaCu/sub 5/ type of crystal structure, particularly LaNiCo/sub 4/ and CaNi/sub 5/, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen cn produce large quantities of heavy water at an effective cost for use in heavy water reactors.

Blind column selection protocol for two-dimensional high performance liquid chromatography.

PubMed

Burns, Niki K; Andrighetto, Luke M; Conlan, Xavier A; Purcell, Stuart D; Barnett, Neil W; Denning, Jacquie; Francis, Paul S; Stevenson, Paul G

2016-07-01

The selection of two orthogonal columns for two-dimensional high performance liquid chromatography (LC×LC) separation of natural product extracts can be a labour intensive and time consuming process and in many cases is an entirely trial-and-error approach. This paper introduces a blind optimisation method for column selection of a black box of constituent components. A data processing pipeline, created in the open source application OpenMS®, was developed to map the components within the mixture of equal mass across a library of HPLC columns; LC×LC separation space utilisation was compared by measuring the fractional surface coverage, fcoverage. It was found that for a test mixture from an opium poppy (Papaver somniferum) extract, the combination of diphenyl and C18 stationary phases provided a predicted fcoverage of 0.48 and was matched with an actual usage of 0.43. OpenMS®, in conjunction with algorithms designed in house, have allowed for a significantly quicker selection of two orthogonal columns, which have been optimised for a LC×LC separation of crude extractions of plant material. Copyright © 2016 Elsevier B.V. All rights reserved.

Use of RSM for the multivariate, simultaneous multiobjective optimization of the operating conditions of aliphatic carboxylic acids ion-exclusion chromatography column: Quantitative study of hydrodynamic, isotherm, and thermodynamic behavior.

PubMed

Shojaeimehr, Tahereh; Rahimpour, Farshad; Schwarze, Michael; Repke, Jens-Uwe; Godini, Hamid Reza; Wozny, Günter

2018-04-15

The present study evaluates the capability of ion exclusion chromatography (IEC) of short chain aliphatic carboxylic acids using a cation exchange column (8% sulfonated cross-linked styrene-divinylbenzene copolymer) in different experimental conditions. Since one of the prerequisites to the development of an efficient carboxylic acid separation process is to obtain the optimum operational conditions, response surface methodology (RSM) was used to develop an approach to evaluate carboxylic acids separation process in IEC columns. The effect of the operating conditions such as column temperature, sulfuric acid concentration as the mobile phase, and the flow rate was studied using Central Composite Face (CCF) design. The optimum operating conditions for the separate injection of lactic acid and acetic acid is temperature of 75 °C, sulfuric acid concentration of 0.003 N for both acids and flow rate of 0.916 (0.886) mL/min for acetic acid (lactic acid). Likewise, the optimum conditions for the simultaneous injection of acetic and lactic acid mixture are the column temperature of 68 °C, sulfuric acid concentration of 0.0003 N, and flow rate of 0.777 mL/min. In the next step, the adsorption equilibria of acetic acid and lactic acid on the stationary phase were investigated through a series of Frontal Analysis (FA), Frontal Analysis by Characteristic Points (FACP), and using Langmuir isotherm model. The results showed an excellent agreement between the model and experimental data. Finally, the results of thermodynamic studies proved that the IEC process for separation of acetic and lactic acid is a spontaneous, feasible, exothermic, and random process with a physical adsorption mechanism. The results of the current paper can be a valuable information in the stages of designing IEC columns for separation of aliphatic carboxylic acids. Copyright © 2018 Elsevier B.V. All rights reserved.

Optimized anion exchange column isolation of zirconium-89 ( 89 Zr) from yttrium cyclotron target: Method development and implementation on an automated fluidic platform

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

O’Hara, Matthew J.; Murray, Nathaniel J.; Carter, Jennifer C.

Zirconium-89 (89Zr), produced by the (p,n) reaction from naturally monoisotopic yttrium (natY), is a promising positron emitting isotope for immunoPET imaging. Its long half-life of 78.4 h is sufficient for evaluating slow physiological processes. A prototype automated fluidic system, coupled to on-line and in-line detectors, has been constructed to facilitate development of new 89Zr purification methodologies. The highly reproducible reagent delivery platform and near-real time monitoring of column effluents allows for efficient method optimization. The separation of Zr from dissolved Y metal targets was evaluated using several anion exchange resins. Each resin was evaluated against its ability to quantitatively capturemore » Zr from a load solution that is high in dissolved Y. The most appropriate anion exchange resin for this application was identified, and the separation method was optimized. The method is capable of a high Y decontamination factor (>105) and has been shown to separate Fe, an abundant contaminant in Y foils, from the 89Zr elution fraction. Finally, the performance of the method was evaluated using cyclotron bombarded Y foil targets. The separation method was shown to achieve >95% recovery of the 89Zr present in the foils. The 89Zr eluent, however, was in a chemical matrix not immediately conducive to labeling onto proteins. The main intent of this study was to develop a tandem column 89Zr purification process, wherein the anion exchange column method described here is the first separation in a dual-column purification process.« less

Comparison of separations of fatty acids from fish products using a 30-m Supelcowax-10 and a 100-m SP-2560 column.

PubMed

Santercole, Viviana; Delmonte, Pierluigi; Kramer, John K G

2012-03-01

Commercial fish oils and foods containing fish may contain trans and/or isomerized fatty acids (FA) produced during processing or as part of prepared foods. The current American Oil Chemists' Society (AOCS) official method for marine oils (method Ce 1i-07) is based on separation by use of poly(ethylene glycol) (PEG) columns, for example Supelcowax-10 or equivalent, which do not resolve most unsaturated FA geometric isomers. Highly polar 100-m cyanopropyl siloxane (CPS) columns, for example SP-2560 and CP Sil 88 are recommended for separation of geometric FA isomers. Complementary separations were achieved by use of two different elution temperature programs with the same CPS column. This study is the first direct comparison of the separations achieved by use of 30-m Supelcowax-10 and 100-m SP-2560 columns for fatty acid methyl esters (FAME) prepared from the same fish oil and fish muscle sample. To simplify the identification of the FA in these fish samples, FA were fractionated on the basis of the number and type of double bonds by silver-ion solid-phase extraction (Ag⁺-SPE) before GC analysis. The results showed that a combination of the three GC separations was necessary to resolve and identify most of the unsaturated FA, FA isomers, and other components of fish products, for example phytanic and phytenic acids. Equivalent chain length (ECL) values of most FAME in fish were calculated from the separations achieved by use of both GC columns; the values obtained were shown to be consistent with previously reported values for the Supelcowax-10 column. ECL values were also calculated for the FA separated on the SP-2560 column. The calculated ECL values were equally valid under isothermal and temperature-programmed elution GC conditions, and were valuable for confirmation of the identity of several unsaturated FAME in the fish samples. When analyzing commercially prepared fish foods, deodorized marine oils, or foods fortified with marine oils it is strongly recommended that quantitative data acquired by use of PEG columns is complemented with data obtained from separations using highly polar CPS columns.

Recent Advances in SRS on Hydrogen Isotope Separation Using Thermal Cycling Absorption Process

DOE PAGES

Xiao, Xin; Sessions, Henry T.; Heung, L. Kit

2015-02-01

The recent Thermal Cycling Absorption Process (TCAP) advances at Savannah River Site (SRS) include compressor-free concept for heating/cooling, push and pull separation using an active inverse column, and compact column design. The new developments allow significantly higher throughput and better reliability from 1/10th of the current production system’s footprint while consuming 60% less energy. Various versions are derived in the meantime for external customers to be used in fusion energy projects and medical isotope production.

Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications.

PubMed

Aral, Tarık; Aral, Hayriye; Ziyadanoğulları, Berrin; Ziyadanoğulları, Recep

2015-01-01

A novel mixed-mode stationary phase was synthesised starting from N-Boc-glutamine, aniline and spherical silica gel (4 µm, 60 Å). The prepared stationary phase was characterized by IR and elemental analysis. The new stationary phase bears an embedded amide group into phenyl ring, highly polar a terminal amide group and non-polar groups (phenyl and alkyl groups). At first, this new mixed-mode stationary phase was used for HILIC separation of four nucleotides and five nucleosides. The effects of different separation conditions, such as pH value, mobile phase and temperature, on the separation process were investigated. The optimum separation for nucleotides was achieved using HILIC isocratic elution with aqueous mobile phase and acetonitrile with 20°C column temperature. Under these conditions, the four nucleotides could be separated and detected at 265 nm within 14 min. Five nucleosides were separated under HILIC isocratic elution with aqueous mobile phase containing pH=3.25 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 265 nm within 14 min. Chromatographic parameters as retention factor, selectivity, theoretical plate number and peak asymmetry factor were calculated for the effect of temperature and water content in mobile phase on the separation process. The new column was also tested for nucleotides and nucleosides mixture and six analytes were separated in 10min. The chromatographic behaviours of these polar analytes on the new mixed-model stationary phase were compared with those of HILIC columns under similar conditions. Further, phytohormones and phenolic compounds were separated in order to see influence of the new stationary phase in reverse phase conditions. Eleven plant phytohormones were separated within 13 min using RP-HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 230 or 278 nm. The best separation conditions for seven phenolic compounds was also achieved using reversed-phase HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and seven phenolic compounds could be separated and detected at 230 nm within 16 min. Copyright © 2014 Elsevier B.V. All rights reserved.

Combined heat and mass transfer device for improving separation process

DOEpatents

Tran, Thanh Nhon

1999-01-01

A two-phase small channel heat exchange matrix simultaneously provides for heat transfer and mass transfer between the liquid and vapor phases of a multi-component mixture at a single, predetermined location within a separation column, significantly improving the thermodynamic efficiency of the separation process. The small channel heat exchange matrix is composed of a series of channels having a hydraulic diameter no greater than 5.0 millimeters for conducting a two-phase coolant. In operation, the matrix provides the liquid-vapor contacting surfaces within the separation column, such that heat and mass are transferred simultaneously between the liquid and vapor phases. The two-phase coolant allows for a uniform heat transfer coefficient to be maintained along the length of the channels and across the surface of the matrix. Preferably, a perforated, concave sheet connects each channel to an adjacent channel to facilitate the flow of the liquid and vapor phases within the column and to increase the liquid-vapor contacting surface area.

Combined heat and mass transfer device for improving separation process

DOEpatents

Tran, T.N.

1999-08-24

A two-phase small channel heat exchange matrix simultaneously provides for heat transfer and mass transfer between the liquid and vapor phases of a multi-component mixture at a single, predetermined location within a separation column, significantly improving the thermodynamic efficiency of the separation process. The small channel heat exchange matrix is composed of a series of channels having a hydraulic diameter no greater than 5.0 millimeters for conducting a two-phase coolant. In operation, the matrix provides the liquid-vapor contacting surfaces within the separation column, such that heat and mass are transferred simultaneously between the liquid and vapor phases. The two-phase coolant allows for a uniform heat transfer coefficient to be maintained along the length of the channels and across the surface of the matrix. Preferably, a perforated, concave sheet connects each channel to an adjacent channel to facilitate the flow of the liquid and vapor phases within the column and to increase the liquid-vapor contacting surface area. 12 figs.

Multiple dual mode counter-current chromatography with variable duration of alternating phase elution steps.

PubMed

Kostanyan, Artak E; Erastov, Andrey A; Shishilov, Oleg N

2014-06-20

The multiple dual mode (MDM) counter-current chromatography separation processes consist of a succession of two isocratic counter-current steps and are characterized by the shuttle (forward and back) transport of the sample in chromatographic columns. In this paper, the improved MDM method based on variable duration of alternating phase elution steps has been developed and validated. The MDM separation processes with variable duration of phase elution steps are analyzed. Basing on the cell model, analytical solutions are developed for impulse and non-impulse sample loading at the beginning of the column. Using the analytical solutions, a calculation program is presented to facilitate the simulation of MDM with variable duration of phase elution steps, which can be used to select optimal process conditions for the separation of a given feed mixture. Two options of the MDM separation are analyzed: 1 - with one-step solute elution: the separation is conducted so, that the sample is transferred forward and back with upper and lower phases inside the column until the desired separation of the components is reached, and then each individual component elutes entirely within one step; 2 - with multi-step solute elution, when the fractions of individual components are collected in over several steps. It is demonstrated that proper selection of the duration of individual cycles (phase flow times) can greatly increase the separation efficiency of CCC columns. Experiments were carried out using model mixtures of compounds from the GUESSmix with solvent systems hexane/ethyl acetate/methanol/water. The experimental results are compared to the predictions of the theory. A good agreement between theory and experiment has been demonstrated. Copyright © 2014 Elsevier B.V. All rights reserved.

CATIONIC EXCHANGE PROCESS FOR THE SEPARATION OF RARE EARTHS

DOEpatents

Choppin, G.R.; Thompson, S.G.; Harvey, B.G.

1960-02-16

A process for separating mixtures of elements in the lanthanum and actinium series of the periodic table is described. The mixture of elements is dissolved in 0.05 M HCI, wherein the elements exist as tripositive ions. The resulting solution is then transferred to a column of cationic exchange resin and the column eluted with 0.1 to 0.6 M aqueous ammonium alpha hydroxy isobutyrate solution of pH 3.8 to 5.0. The use of ammonium alpha hydroxy isobutyrate as an eluting agent results in sharper and more rapid separations than previously obtainable with eluants such as citric, tartaric, glycolic, and lactic acids.

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 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.

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.

Continuous separation of copper ions from a mixture of heavy metal ions using a three-zone carousel process packed with metal ion-imprinted polymer.

PubMed

Jo, Se-Hee; Lee, See-Young; Park, Kyeong-Mok; Yi, Sung Chul; Kim, Dukjoon; Mun, Sungyong

2010-11-05

In this study, a three-zone carousel process based on a proper molecular imprinted polymer (MIP) resin was developed for continuous separation of Cu(2+) from Mn(2+) and Co(2+). For this task, the Cu (II)-imprinted polymer (Cu-MIP) resin was synthesized first and used to pack the chromatographic columns of a three-zone carousel process. Prior to the experiment of the carousel process based on the Cu-MIP resin (MIP-carousel process), a series of single-column experiments were performed to estimate the intrinsic parameters of the three heavy metal ions and to find out the appropriate conditions of regeneration and re-equilibration. The results from these single-column experiments and the additional computer simulations were then used for determination of the operating parameters of the MIP-carousel process under consideration. Based on the determined operating parameters, the MIP-carousel experiments were carried out. It was confirmed from the experimental results that the proposed MIP-carousel process was markedly effective in separating Cu(2+) from Mn(2+) and Co(2+) in a continuous mode with high purity and a relatively small loss. Thus, the MIP-carousel process developed in this study deserves sufficient attention in materials processing industries or metal-related industries, where the selective separation of heavy metal ions with the same charge has been a major concern. Copyright © 2010 Elsevier B.V. All rights reserved.

[Determination of sennosides and degraded products in the process of sennoside metabolism by HPLC].

PubMed

Sun, Yan; Li, Xuetuo; Yu, Xingju

2004-01-01

A method for the separation and determination of sennosides A and B and the main composition (sennidins A and B) in degraded products of sennosides by linear gradient high performance liquid chromatography has been developed. Separation conditions were as follows: column, a Spherisorb C18 column (250 mm x 4.6 mm i.d., 10 microm); column temperature, 40 degrees C; detection wavelength, 360 nm; mobile phase A, 1.25% acetic acid aqueous solution; mobile phase B, methanol; linear gradient, 100% A --> (20 min) 100% B. The method is effective, quick, accurate and reproducible. The satisfactory results show that this new method has certain practical values as an approach of real-time analysis in the process of sennoside metabolism.

Continuous countercurrent membrane column for the separation of solute/solvent and solvent/solvent systems

DOEpatents

Nerad, Bruce A.; Krantz, William B.

1988-01-01

A reverse osmosis membrane process or hybrid membrane - complementary separator process for producing enriched product or waste streams from concentrated and dilute feed streams for both solvent/solvent and solute/solvent systems is described.

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.

INTERIOR VIEW OF FILTER WHEEL MACHINE USED TO FILTER OUT ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

INTERIOR VIEW OF FILTER WHEEL MACHINE USED TO FILTER OUT AND SEPARATE BICARBONATE FROM AMMONIONATED BRINE. DISCHARGE FROM STRIPPER COLUMNS (SOLVAY COLUMNS). - Solvay Process Company, SA Wetside Building, Between Willis & Milton Avenue, Solvay, Onondaga County, NY

Scale-up protein separation on stainless steel wide bore toroidal columns in the type-J counter-current chromatography.

PubMed

Guan, Yue Hugh; Hewitson, Peter; van den Heuvel, Remco N A M; Zhao, Yan; Siebers, Rick P G; Zhuang, Ying-Ping; Sutherland, Ian

2015-12-11

Manufacturing high-value added biotech biopharmaceutical products (e.g. therapeutic proteins) requires quick-to-develop, GMP-compliant, easy-to-scale and cost effective preparatory chromatography technologies. In this work, we describe the construction and testing of a set of 5-mm inner diameter stainless steel toroidal columns for use on commercially available preparatory scale synchronous J-type counter-current chromatography (CCC) machinery. We used a 20.2m long column with an aqueous two-phase system containing 14% (w/w) PEG1000 and 14% (w/w) potassium phosphate at pH 7, and tested a sample loading of 5% column volume and a mobile phase flow rate of 20ml/min. We then satisfactorily demonstrated the potential for a weekly protein separation and preparation throughput of ca. 11g based on a normal weekly routine for separating a pair of model proteins by making five stacked injections on a single portion of stationary phase with no stripping. Compared to our previous 1.6mm bore PTFE toroidal column, the present columns enlarged the nominal column processing throughput by nearly 10. For an ideal model protein injection modality, we observed a scaling up factor of at least 21. The 2 scales of protein separation and purification steps were realized on the same commercial CCC device. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

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.

INTERIOR VIEW FROM CATWALKS LOOKING DOWN ON FILTER WHEEL MACHINES. ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

INTERIOR VIEW FROM CATWALKS LOOKING DOWN ON FILTER WHEEL MACHINES. USED TO FILTER OUT AND SEPARATE BICARBONATE FROM AMMONIONATED BRINE. DISCHARGE FROM STRIPPER COLUMNS (SOLVAY COLUMNS). - Solvay Process Company, SA Wetside Building, Between Willis & Milton Avenue, Solvay, Onondaga County, NY

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.

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

Youker, Amanda J.; Krebs, John F.; Quigley, Kevin J.

With funding from the National Nuclear Security Administrations Material Management and Minimization Office, Argonne National Laboratory (Argonne) is providing technical assistance to help accelerate the U.S. production of Mo-99 using a non-highly enriched uranium (non-HEU) source. A potential Mo-99 production pathway is by accelerator-initiated fissioning in a subcritical uranyl sulfate solution containing low enriched uranium (LEU). As part of the Argonne development effort, we are undertaking the AMORE (Argonne Molybdenum Research Experiment) project, which is essentially a pilot facility for all phases of Mo-99 production, recovery, and purification. Production of Mo-99 and other fission products in the subcritical target solutionmore » is initiated by putting an electron beam on a depleted uranium (DU) target; the fast neutrons produced in the DU target are thermalized and lead to fissioning of U-235. At the end of irradiation, Mo is recovered from the target solution and separated from uranium and most of the fission products by using a titania column. The Mo is stripped from the column with an alkaline solution. After acidification of the Mo product solution from the recovery column, the Mo is concentrated (and further purified) in a second titania column. The strip solution from the concentration column is then purified with the LEU Modified Cintichem process. A full description of the process can be found elsewhere [1–3]. The initial commissioning steps for the AMORE project include performing a Mo-99 spike test with pH 1 sulfuric acid in the target vessel without a beam on the target to demonstrate the initial Mo separation-and-recovery process, followed by the concentration column process. All glovebox operations were tested with cold solutions prior to performing the Mo-99 spike tests. Two Mo-99 spike tests with pH 1 sulfuric acid have been performed to date. Figure 1 shows the flow diagram for the remotely operated Mo-recovery system for the AMORE project. There are two separate pumps and flow paths for the acid and base operations. The system contains three sample ladders with eight sample loops per ladder for target mixing; column loading, including acid and water washes; and column stripping, including the final water wash.« less

The setup of an extraction system coupled to a hydrogen isotopes distillation column

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

Zamfirache, M.; Bornea, A.; Stefanescu, I.

2008-07-15

Among the most difficult problems of cryogenic distillation one stands apart: the extraction of the heavy fraction. By an optimal design of the cycle scheme, this problem could be avoided. A 'worst case scenario' is usually occurring when the extracted fraction consists of one prevalent isotope such as hydrogen and small amounts of the other two hydrogen isotopes (deuterium and/or tritium). This situation is further complicated by two parameters of the distillation column: the extraction flow rate and the hold-up. The present work proposes the conceptual design of an extraction system associated to the cryogenic distillation column used in hydrogenmore » separation processes. During this process, the heavy fraction (DT, T{sub 2}) is separated, its concentration being the highest at the bottom of the distillation column. From this place the extraction of the gaseous phase can now begin. Being filled with adsorbent, the extraction system is used to temporarily store the heavy fraction. Also the extraction system provides samples for the gas Chromatograph. The research work is focused on the existent pilot plant for tritium and deuterium separation from our institute to validate the experiments carried out until now. (authors)« less

REDISTRIBUTOR FOR LIQUID-LIQUID EXTRACTION COLUMNS

DOEpatents

Bradley, J.G.

1957-10-29

An improved baffle plate construction to intimately mix immiscible liquid solvents for solvent extraction processes in a liquid-liquid pulse column is described. To prevent the light and heavy liquids from forming separate continuous homogeneous vertical channels through sections of the column, a baffle having radially placed rectangular louvers with deflection plates opening upon alternate sides of the baffle is placed in the column, normal to the axis. This improvement substantially completely reduces strippiig losses due to poor mixing.

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.

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.

Tunable thick porous silica coating fabricated by multilayer-by-multilayer bonding of silica nanoparticles for open-tubular capillary chromatographic separation.

PubMed

Qu, Qishu; Liu, Yuanyuan; Shi, Wenjun; Yan, Chao; Tang, Xiaoqing

2015-06-19

A simple coating procedure employing a multilayer-by-multilayer process to modify the inner surface of bare fused-silica capillaries with silica nanoparticles was established. The silica nanoparticles were adsorbed onto the capillary wall via a strong electrostatic interaction between amino functional groups and silica particles. The thickness of the coating could be tuned from 130 to 600 nm by increasing the coating cycles from one to three. Both the retention factor and the resolution were greatly increased with increasing coating cycles. The loading capacity determined by naphthalene in the column with three coating cycles is 152.1 pmol. The effects of buffer concentration and pH value on the stability of the coating were evaluated. The retention reproducibility of the separation of toluene was 0.8, 1.2, 2.3, and 4.5%, respectively, for run-to-run, day-to-day, column-to-column, and batch-to-batch, respectively. The chromatographic performance of these columns was evaluated by both capillary liquid chromatography and open-tubular capillary electrochromatography (OT-CEC). Separation of aromatic hydrocarbons in the column with three coating cycles provided high theoretical plate numbers (up to 269,280 plates m(-1) for toluene) and short separation time (<15 min) by using OT-CEC mode. The method was also used to separate egg white proteins. Both acidic and basic proteins as well as four glycoisoforms were separated in a single run. Copyright © 2015 Elsevier B.V. All rights reserved.

Separation of copper, iron, and zinc from complex aqueous solutions for isotopic measurement

USGS Publications Warehouse

Borrok, D.M.; Wanty, R.B.; Ridley, W.I.; Wolf, R.; Lamothe, P.J.; Adams, M.

2007-01-01

The measurement of Cu, Fe, and Zn isotopes in natural samples may provide valuable information about biogeochemical processes in the environment. However, the widespread application of stable Cu, Fe, and Zn isotope chemistry to natural water systems remains limited by our ability to efficiently separate these trace elements from the greater concentrations of matrix elements. In this study, we present a new method for the isolation of Cu, Fe, and Zn from complex aqueous solutions using a single anion-exchange column with hydrochloric acid media. Using this method we are able to quantitatively separate Cu, Fe, and Zn from each other and from matrix elements in a single column elution. Elution of the elements of interest, as well as all other elements, through the anion-exchange column is a function of the speciation of each element in the various concentrations of HCl. We highlight the column chemistry by comparing our observations with published studies that have investigated the speciation of Cu, Fe, and Zn in chloride solutions. The functionality of the column procedure was tested by measuring Cu, Fe, and Zn isotopes in a variety of stream water samples impacted by acid mine drainage. The accuracy and precision of Zn isotopic measurements was tested by doping Zn-free stream water with the Zn isotopic standard. The reproducibility of the entire column separation process and the overall precision of the isotopic measurements were also evaluated. The isotopic results demonstrate that the Cu, Fe, and Zn column separates from the tested stream waters are of sufficient purity to be analyzed directly using a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS), and that the measurements are fully-reproducible, accurate, and precise. Although limited in scope, these isotopic measurements reveal significant variations in ??65Cu (- 1.41 to + 0.30???), ??56Fe (- 0.56 to + 0.34???), and ??66Zn (0.31 to 0.49???) among samples collected from different abandoned mines within a single watershed. Hence, Cu, Fe, and Zn isotopic measurements may be a powerful tool for fingerprinting specific metal sources and/or examining biogeochemical reactions within fresh water systems.

Separations on water-ice. Final report

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

Dasgupta, P.K.

1998-07-01

This report focuses on processes to separate water frozen into ice. Research topics include the following: normal phase columnar chromatography; electrophoresis in a planar format; and zone melting type separations on a solid column of ice. Attempts were made to dope the emulsion with {beta}-cyclodextrin in order to separate commercially important chiral drugs such as Inderal.

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.

Enantioseparation on cellulose dimethylphenylcarbamate-modified zirconia monolithic columns by reversed-phase capillary electrochromatography.

PubMed

Kumar, Avvaru Praveen; Park, Jung Hag

2010-06-25

This work reports the preparation of monolithic zirconia chiral columns for separation of enantiomeric compounds by capillary electrochromatography (CEC). Using sol-gel technology, a porous monolith having interconnected globular-like structure with through-pores is synthesized in the capillary column as a first step in the synthesis of monolithic zirconia chiral capillary columns. In the second step, the surface of the monolith is modified by coating with cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) as the chiral stationary phase to obtain a chiral column (CDMPCZM). The process of the preparation of the zirconia monolithic capillary column was investigated by varying the concentrations of the components of the sol solution including polyethylene glycol, water and acetic acid. CDMPCZM is mechanically stable and no bubble formation was detected with the applied current of up to 30 microA. The enantioseparation behavior of the CDMPCZM columns was investigated by separating a set of 10 representative chiral compounds by varying the applied voltage and pH and organic composition of the aqueous organic mobile phases. Copyright 2010 Elsevier B.V. All rights reserved.

Practical comparison of 2.7 microm fused-core silica particles and porous sub-2 microm particles for fast separations in pharmaceutical process development.

PubMed

Abrahim, Ahmed; Al-Sayah, Mohammad; Skrdla, Peter; Bereznitski, Yuri; Chen, Yadan; Wu, Naijun

2010-01-05

Fused-core silica stationary phases represent a key technological advancement in the arena of fast HPLC separations. These phases are made by fusing a 0.5 microm porous silica layer onto 1.7 microm nonporous silica cores. The reduced intra-particle flow path of the fused particles provides superior mass transfer kinetics and better performance at high mobile phase velocities, while the fused-core particles provide lower pressure than sub-2 microm particles. In this work, chromatographic performance of the fused-core particles (Ascentis Express) was investigated and compared to that of sub-2 microm porous particles (1.8 microm Zorbax Eclipse Plus C18 and 1.7 microm Acquity BEH C18). Specifically, retention, selectivity, and loading capacity were systematically compared for these two types of columns. Other chromatographic parameters such as efficiency and pressure drop were also studied. Although the fused-core column was found to provide better analyte shape selectivity, both columns had similar hydrophobic, hydrogen bonding, total ion-exchange, and acidic ion-exchange selectivities. As expected, the retention factors and sample loading capacity on the fused-core particle column were slightly lower than those for the sub-2 microm particle column. However, the most dramatic observation was that similar efficiency separations to the sub-2 microm particles could be achieved using the fused-core particles, without the expense of high column back pressure. The low pressure of the fused-core column allows fast separations to be performed routinely on a conventional LC system without significant loss in efficiency or resolution. Applications to the HPLC impurity profiling of drug substance candidates were performed using both types of columns to validate this last point.

Preparation of a novel dual-function strong cation exchange/hydrophobic interaction chromatography stationary phase for protein separation.

PubMed

Zhao, Kailou; Yang, Li; Wang, Xuejiao; Bai, Quan; Yang, Fan; Wang, Fei

2012-08-30

We have explored a novel dual-function stationary phase which combines both strong cation exchange (SCX) and hydrophobic interaction chromatography (HIC) characteristics. The novel dual-function stationary phase is based on porous and spherical silica gel functionalized with ligand containing sulfonic and benzyl groups capable of electrostatic and hydrophobic interaction functionalities, which displays HIC character in a high salt concentration, and IEC character in a low salt concentration in mobile phase employed. As a result, it can be employed to separate proteins with SCX and HIC modes, respectively. The resolution and selectivity of the dual-function stationary phase were evaluated under both HIC and SCX modes with standard proteins and can be comparable to that of conventional IEC and HIC columns. More than 96% of mass and bioactivity recoveries of proteins can be achieved in both HIC and SCX modes, respectively. The results indicated that the novel dual-function column could replace two individual SCX and HIC columns for protein separation. Mixed retention mechanism of proteins on this dual-function column based on stoichiometric displacement theory (SDT) in LC was investigated to find the optimal balance of the magnitude of electrostatic and hydrophobic interactions between protein and the ligand on the silica surface in order to obtain high resolution and selectivity for protein separation. In addition, the effects of the hydrophobicity of the ligand of the dual-function packings and pH of the mobile phase used on protein separation were also investigated in detail. The results show that the ligand with suitable hydrophobicity to match the electrostatic interaction is very important to prepare the dual-function stationary phase, and a better resolution and selectivity can be obtained at pH 6.5 in SCX mode. Therefore, the dual-function column can replace two individual SCX and HIC columns for protein separation and be used to set up two-dimensional liquid chromatography with a single column (2DLC-1C), which can also be employed to separate three kinds of active proteins completely, such as lysozyme, ovotransferrin and ovalbumin from egg white. The result is very important not only to the development of new 2DLC technology with a single column for proteomics, but also to recombinant protein drug production for saving column expense and simplifying the process in biotechnology. Copyright © 2012 Elsevier B.V. All rights reserved.

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.

The Application of TD/GC/NICI-MS with an Al2O3-PLOT-S Column for the Determination of Perfluoroalkylcycloalkanes in the Atmosphere.

PubMed

Ren, Yu; Schlager, Hans; Martin, Damien

2014-01-01

A modified method for the quantitative determination of atmospheric perfluoroalkylcycloalkanes (PFCs) using thermal desorption coupled with gas chromatography and detection by negative ion chemical ionization-mass spectrometry was developed. Using an optimized analytical system, a commercially available Al 2 O 3 porous layer open tubular (PLOT) capillary column (30 m × 0.25 mm) deactivated with Na 2 SO 4 was used for separation of PFCs. Improvements in the separation of PFCs, the corresponding identification and the limit of detection of PFCs using this method and column are presented. The method was successfully applied to determine the atmospheric background concentrations of a range of PFCs from a number of samples collected at a rural site in Germany. The results of this study suggest that the method outlined using the Al 2 O 3 -PLOT-S capillary column has good sensitivity and selectivity, and that it can be deployed in a routine laboratory process for the analysis of PFCs in the future research work. In addition, the ability of this column to separate the isomers of one of the lower boiling PFCs (perfluorodimethylcyclobutane) and its ability to resolve perfluoroethylcyclohexane offer the opportunity for single-column analysis for multiple PFCs.

Separation of natural product using columns packed with Fused-Core particles.

PubMed

Yang, Peilin; Litwinski, George R; Pursch, Matthias; McCabe, Terry; Kuppannan, Krishna

2009-06-01

Three HPLC columns packed with 3 microm, sub-2 microm, and 2.7 microm Fused-Core (superficially porous) particles were compared in separation performance using two natural product mixtures containing 15 structurally related components. The Ascentis Express C18 column packed with Fused-Core particles showed an 18% increase in column efficiency (theoretical plates), a 76% increase in plate number per meter, a 65% enhancement in separation speed and a 19% increase in back pressure compared to the Atlantis T3 C18 column packed with 3 microm particles. Column lot-to-lot variability for critical pairs in the natural product mixture was observed with both columns, with the Atlantis T3 column exhibiting a higher degree of variability. The Ascentis Express column was also compared with the Acquity BEH column packed with sub-2 microm particles. Although the peak efficiencies obtained by the Ascentis Express column were only about 74% of those obtained by the Acquity BEH column, the 50% lower back pressure and comparable separation speed allowed high-efficiency and high-speed separation to be performed using conventional HPLC instrumentation.

Silver ion chromatography for peak resolution enhancement: Application to the preparative separation of two sesquiterpenes using online heart-cutting LC-LC technique.

PubMed

Yang, Yang; Zhang, Yongmin; Wei, Chong; Li, Jing; Sun, Wenji

2018-09-01

Silver ion chromatography, utilizing columns packed with silver ions bonded to silica gel, has proved to be an invaluable technique for the analysis of some positional isomers. In this work, silver ion chromatography by combination with online heart-cutting LC-LC technique for the preparative separation of two sesquiterpenes positional isomers from a natural product was investigated. On the basis of the evaluation that silver ion content impacts on the separation, the laboratory-made silver ion columns, utilizing silica gel impregnated with 15% silver nitrate as column packing materials, were used for peak resolution improvement of these two isomers and the preparative separation of them in heart-cutting LC-LC. The relationship among the maximal sample load, flow rate and peak resolution in the silver ion column were optimized, and the performance of the silver ion column was compared with conventional C 18 column and silica gel column. Based on the developed chromatographic conditions, online heart-cutting LC-LC chromatographic separation system in combination with a silica gel column and a silver ion column that was applied to preparative separation of these two isomers from a traditional Chinese medicine, Inula racemosa Hook.f., was established. The results showed that the online heart-cutting LC-LC technique by combination of a silica gel column and a silver ion column for the preparative separation of these two positional isomers from this natural plant was superior to the preparative separation performed on a single-column system with C 18 column or silica gel column. Copyright © 2018 Elsevier B.V. All rights reserved.

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

PubMed Central

Heshka, Nicole E.; Hager, Darcy B.

2015-01-01

A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate interferences, a two dimensional column configuration is used, with a Deans switch employed to transfer hydrogen sulfide from the first to the second column (heart-cutting). Liquid crude samples are first separated on a dimethylpolysiloxane column, and light gases are heart-cut and further separated on a bonded porous layer open tubular (PLOT) column that is able to separate hydrogen sulfide from other light sulfur species. Hydrogen sulfide is then detected with a sulfur chemiluminescence detector, adding an additional layer of selectivity. Following separation and detection of hydrogen sulfide, the system is backflushed to remove the high-boiling hydrocarbons present in the crude samples and to preserve chromatographic integrity. Dissolved hydrogen sulfide has been quantified in liquid samples from 1.1 to 500 ppm, demonstrating wide applicability to a range of samples. The method has also been successfully applied for the analysis of gas samples from crude oil headspace and process gas bags, with measurement from 0.7 to 9,700 ppm hydrogen sulfide. PMID:26709594

Modelling aspects regarding the control in 13C isotope separation column

NASA Astrophysics Data System (ADS)

Boca, M. L.

2016-08-01

Carbon represents the fourth most abundant chemical element in the world, having two stable and one radioactive isotope. The 13Carbon isotopes, with a natural abundance of 1.1%, plays an important role in numerous applications, such as the study of human metabolism changes, molecular structure studies, non-invasive respiratory tests, Alzheimer tests, air pollution and global warming effects on plants [9] A manufacturing control system manages the internal logistics in a production system and determines the routings of product instances, the assignment of workers and components, the starting of the processes on not-yet-finished product instances. Manufacturing control does not control the manufacturing processes themselves, but has to cope with the consequences of the processing results (e.g. the routing of products to a repair station). In this research it was fulfilled some UML (Unified Modelling Language) diagrams for modelling the C13 Isotope Separation column, implement in STARUML program. Being a critical process and needing a good control and supervising, the critical parameters in the column, temperature and pressure was control using some PLC (Programmable logic controller) and it was made some graphic analyze for this to observe some critical situation than can affect the separation process. The main parameters that need to be control are: -The liquid nitrogen (N2) level in the condenser. -The electrical power supplied to the boiler. -The vacuum pressure.

Separation of carbon nanotubes into chirally enriched fractions

DOEpatents

Doorn, Stephen K [Los Alamos, NM; Niyogi, Sandip [Los Alamos, NM

2012-04-10

A mixture of single-walled carbon nanotubes ("SWNTs") is separated into fractions of enriched chirality by preparing an aqueous suspension of a mixture of SWNTs and a surfactant, injecting a portion of the suspension on a column of separation medium having a density gradient, and centrifuging the column. In some embodiments, salt is added prior to centrifugation. In other embodiments, the centrifugation is performed at a temperature below room temperature. Fractions separate as colored bands in the column. The diameter of the separated SWNTs decreases with increasing density along the gradient of the column. The colored bands can be withdrawn separately from the column.

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 PROCESS FOR SEPARATING AZEOTROPIC MIXTURES BY EXTRACTIVE AND CONVECTIVE DISTILLATION

DOEpatents

Frazer, J.W.

1961-12-19

A method is described for separating an azeotrope of carbon tetrachloride and 1,1,2,2-tetrafluorodinitroethane boiling at 60 deg C. The ndethod comnprises, specifically, feeding azeotrope vapors admixed with a non- reactive gas into an extractive distillation column heated to a temperature preferably somewhat above the boiling point of the constant boiling mixture. A solvent, di-n-butylphthalate, is metered into the column above the gas inlet and permitted to flow downward, earrying with it the higher bomling fraction, while the constituent having the lower boiling point passes out of the top of the column with the non-reactive gas and is collected in a nitrogen cold trap. Other solvents which alter the vapor pressure relationship may be substituted. The method is generally applicable to azeotropic mixtures. A number of specific mixtures whicb may be separated are disclosed. (AEC)

Systems for column-based separations, methods of forming packed columns, and methods of purifying sample components

DOEpatents

Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

2000-01-01

The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

Systems For Column-Based Separations, Methods Of Forming Packed Columns, And Methods Of Purifying Sample Components

DOEpatents

Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

2006-02-21

The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

Systems For Column-Based Separations, Methods Of Forming Packed Columns, And Methods Of Purifying Sample Components.

DOEpatents

Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

2004-08-24

The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

A simple and inexpensive on-column frit fabrication method for fused-silica capillaries for increased capacity and versatility in LC-MS/MS applications.

PubMed

Wang, Ling-Chi; Okitsu, Cindy Yen; Kochounian, Harold; Rodriguez, Anthony; Hsieh, Chih-Lin; Zandi, Ebrahim

2008-05-01

A modified sol-gel method for a one-step on-column frit preparation for fused-silica capillaries and its utility for peptide separation in LC-MS/MS is described. This method is inexpensive, reproducible, and does not require specialized equipments. Because the frit fabrication process does not damage polyimide coating, the frit-fabricated column can be tightly connected on-line for high pressure LC. These columns can replace any capillary liquid transfer tubing without any specialized connections up-stream of a spray tip column. Therefore multiple columns with different phases can be connected in series for one- or multiple-dimensional chromatography.

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 Effect of Column and Eluent Fluorination on the Retention and Separation of non-Fluorinated Amino Acids and Proteins by HPLC

PubMed Central

Joyner, Katherine; Wang, Weizhen; Yu, Yihua Bruce

2011-01-01

The effect of column and eluent fluorination on the retention and separation of non-fluorinated amino acids and proteins in HPLC is investigated. A side-by-side comparison of fluorocarbon column and eluents (F-column and F-eluents) with their hydrocarbon counterparts (H-column and H-eluents) in the separation of a group of 33 analytes, including 30 amino acids and 3 proteins, is conducted. The H-column and the F-column contain the n-C8H17 group and n-C8F17 group, respectively, in their stationary phases. The H-eluents include ethanol (EtOH) and isopropanol (ISP) while the F-eluents include trifluoroethanol (TFE) and hexafluorosopropanol (HFIP). The 2 columns and 4 eluents generated 8 (column, eluent) pairs that produce 264 retention time data points for the 33 analytes. A statistical analysis of the retention time data reveals that although the H-column is better than the F-column in analyte separation and H-eluents are better than F-eluents in analyte retention, the more critical factor is the proper pairing of column with eluent. Among the conditions explored in this project, optimal retention and separation is achieved when the fluorocarbon column is paired with ethanol, even though TFE is the most polar one among the 4 eluents. This result shows fluorocarbon columns have much potential in chromatographic analysis and separation of non-fluorinated amino acids and proteins. PMID:21318121

Evaluation of reversible interconversion in comprehensive two-dimensional gas chromatography using enantioselective columns in first and second dimensions.

PubMed

Kröger, Sabrina; Wong, Yong Foo; Chin, Sung-Tong; Grant, Jacob; Lupton, David; Marriott, Philip J

2015-07-24

The reversible molecular interconversion behaviour of a synthesised oxime (2-phenylpropanaldehyde oxime; (C6H5)CH(CH3)CHN(OH)) was investigated by both, single dimensional gas chromatography (1D GC) and comprehensive two-dimensional gas chromatography (GC×GC). Previous studies on small molecular weight oximes were extended to this larger aromatic oxime (molar mass 149.19gmol(-1)) with interest in the extent of interconversion, enantioselective resolution, and retention time. On a polyethylene glycol (PEG; wax-type) column, a characteristic interconversion zone between two antipodes of E and Z isomers was formed by molecules which have undergone isomerisation on the column (E⇌Z). The extent of interconversion was investigated by varying chromatographic conditions (oven temperature and carrier flow rate) to understand the nature of the behaviour observed. The extent of interconversion was negligible in both enantioselective and methyl-phenylpolysiloxane phase-columns, correlating with the low polarity of the stationary phase. In order to obtain isomerisation along with enantio-resolution, a wax-type and an enantioselective column were coupled in either enantioselective-wax or wax-enantioselective order. The most appropriate column arrangement was selected for study by using a GC×GC experiment with either a wax-phase or phenyl-methylpolysiloxane phase as (2)D column. In addition to evaluation of these fast elution columns, a long narrow-bore enantioselective column (10m) was introduced as (2)D, providing an enantioselective-PEG (coupled-column ensemble: (1)D1+(1)D2)×enantioselective ((2)D) column combination. In this instance, the (1)D1 enantioselective column provides enantiomeric separation of the corresponding enantiomers ((R) and (S)) of (E)- and (Z)-2-phenylpropanaldehyde oxime, followed by E/Z isomerisation in the coupled (1)D2 PEG (reactor) column. The resulting chromatographic interconversion region was modulated and separated into either E/Z isomers (achiral (2)D column) or into the respective (R) and (S) enantiomers of the E/Z isomers when using a (2)D enantioselective column. With this arrangement, the isomers underneath the broad interconversion plateau in 1D elution profiles, including the enantiomers, could be resolved, illuminating salient features and understanding of the molecular reversible process of the interconverting molecules during the chromatographic elution. The two-dimensional patterns (contour plots), resulting from the combination of interconversion process and chiral separation, are discussed phenomenologically. Copyright © 2015 Elsevier B.V. All rights reserved.

Evaluation of chromatographic columns packed with semi- and fully porous particles for benzimidazoles separation.

PubMed

Gonzalo-Lumbreras, Raquel; Sanz-Landaluze, Jon; Cámara, Carmen

2015-07-01

The behavior of 15 benzimidazoles, including their main metabolites, using several C18 columns with standard or narrow-bore diameters and different particle size and type were evaluated. These commercial columns were selected because their differences could affect separation of benzimidazoles, and so they can be used as alternative columns. A simple screening method for the analysis of benzimidazole residues and their main metabolites was developed. First, the separation of benzimidazoles was optimized using a Kinetex C18 column; later, analytical performances of other columns using the above optimized conditions were compared and then individually re-optimized. Critical pairs resolution, analysis run time, column type and characteristics, and selectivity were considered for chromatographic columns comparison. Kinetex XB was selected because it provides the shortest analysis time and the best resolution of critical pairs. Using this column, the separation conditions were re-optimized using a factorial design. Separations obtained with the different columns tested can be applied to the analysis of specific benzimidazoles residues or other applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of the separation characteristics of application-specific (volatile organic compounds) open-tubular columns for gas chromatography.

PubMed

Poole, Colin F; Qian, Jing; Kiridena, Waruna; Dekay, Colleen; Koziol, Wladyslaw W

2006-11-17

The solvation parameter model is used to characterize the separation characteristics of two application-specific open-tubular columns (Rtx-Volatiles and Rtx-VGC) and a general purpose column for the separation of volatile organic compounds (DB-WAXetr) at five equally spaced temperatures over the range 60-140 degrees C. System constant differences and retention factor correlation plots are then used to determine selectivity differences between the above columns and their closest neighbors in a large database of system constants and retention factors for forty-four open-tubular columns. The Rtx-Volatiles column is shown to have separation characteristics predicted for a poly(dimethyldiphenylsiloxane) stationary phase containing about 16% diphenylsiloxane monomer. The Rtx-VGC column has separation properties similar to the poly(cyanopropylphenyldimethylsiloxane) stationary phase containing 14% cyanopropylphenylsiloxane monomer DB-1701 for non-polar and dipolar/polarizable compounds but significantly different characteristics for the separation of hydrogen-bond acids. For all practical purposes the DB-WAXetr column is shown to be selectivity equivalent to poly(ethylene glycol) columns prepared using different chemistries for bonding and immobilizing the stationary phase. Principal component analysis and cluster analysis are then used to classify the system constants for the above columns and a sub-database of eleven open-tubular columns (DB-1, HP-5, DB-VRX, Rtx-20, DB-35, Rtx-50, Rtx-65, DB-1301, DB-1701, DB-200, and DB-624) commonly used for the separation of volatile organic compounds. A rationale basis for column selection based on differences in intermolecular interactions is presented as an aid to method development for the separation of volatile organic compounds.

Multi-Column Experimental Test Bed Using CaSDB MOF for Xe/Kr Separation

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

Welty, Amy Keil; Greenhalgh, Mitchell Randy; Garn, Troy Gerry

Processing of spent nuclear fuel produces off-gas from which several volatile radioactive components must be separated for further treatment or storage. As part of the Off-gas Sigma Team, parallel research at INL and PNNL has produced several promising sorbents for the selective capture of xenon and krypton from these off-gas streams. In order to design full-scale treatment systems, sorbents that are promising on a laboratory scale must be proven under process conditions to be considered for pilot and then full-scale use. To that end, a bench-scale multi-column system with capability to test multiple sorbents was designed and constructed at INL.more » This report details bench-scale testing of CaSDB MOF, produced at PNNL, and compares the results to those reported last year using INL engineered sorbents. Two multi-column tests were performed with the CaSDB MOF installed in the first column, followed with HZ-PAN installed in the second column. The CaSDB MOF column was placed in a Stirling cryocooler while the cryostat was employed for the HZ-PAN column. Test temperatures of 253 K and 191 K were selected for the first column while the second column was held at 191 K for both tests. Calibrated volume sample bombs were utilized for gas stream analyses. At the conclusion of each test, samples were collected from each column and analyzed for gas composition. While CaSDB MOF does appear to have good capacity for Xe, the short time to initial breakthrough would make design of a continuous adsorption/desorption cycle difficult, requiring either very large columns or a large number of smaller columns. Because of the tenacity with which Xe and Kr adhere to the material once adsorbed, this CaSDB MOF may be more suitable for use as a long-term storage solution. Further testing is recommended to determine if CaSDB MOF is suitable for this purpose.« less

Separation and Detection of Toxic Gases with a Silicon Micromachined Gas Chromatography System

NASA Technical Reports Server (NTRS)

Kolesar, Edward S.; Reston, Rocky R.

1995-01-01

A miniature gas chromatography (GC) system was designed and fabricated using silicon micromachining and integrated circuit (IC) processing techniques. The silicon micromachined gas chromatography system (SMGCS) is composed of a miniature sample injector that incorporates a 10 microliter sample loop; a 0.9 meter long, rectangular shaped (300 micrometer width and 10 micrometer height) capillary column coated with a 0.2 micrometer thick copper phthalocyanine (CuPc) stationary phase; and a dual detector scheme based upon a CuPc-coated chemiresistor and a commercially available 125 micrometer diameter thermal conductivity detector (TCD) bead. Silicon micromachining was employed to fabricate the interface between the sample injector and the GC column, the column itself, and the dual detector cavity. A novel IC thin-film processing technique was developed to sublime the CuPc stationary phase coating on the column walls that were micromachined in the host silicon wafer substrate and Pyrex (r) cover plate, which were then electrostatically bonded together. The SMGCS can separate binary gas mixtures composed of parts-per-million (ppm) concentrations of ammonia (NH3) and nitrogen dioxide (NO2) when isothermally operated (55-80 degrees C). With a helium carrier gas and nitrogen diluent, a 10 microliter sample volume containing ammonia and nitrogen dioxide injected at 40 psi ((2.8 x 10(exp 5)Pa)) can be separated in less than 30 minutes.

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.

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

Bornea, A.; Zamfirache, M.; Stefan, L.

ICIT (Institute for Cryogenics and Isotopic Technologies) has used its experience in cryogenic water distillation process to propose a similar process for hydrogen distillation that can be used in detritiation technologies. This process relies on the same packages but a stainless filling is tested instead of the phosphorous bronze filling used for water distillation. This paper presents two types of packages developed for hydrogen distillation, both have a stainless filling but it differs in terms of density, exchange surface and specific volume. Performance data have been obtained on laboratory scale. In order to determine the characteristics of the package, themore » installation was operated in the total reflux mode, for different flow rate for the liquid. There were made several experiments considering different operating conditions. Samples extracted at the top and bottom of cryogenic distillation column allowed mathematical processing to determine the separation performance. The experiments show a better efficiency for the package whose exchange surface was higher and there were no relevant differences between both packages as the operating pressure of the cryogenic column was increasing. For a complete characterization of the packages, future experiments will be considered to determine performance at various velocities in the column and their correlation with the pressure in the column. We plan further experiments to separate tritium from the mixture of isotopes DT, having in view that our goal is to apply this results to a detritiation plant.« less

Evaluation of separation properties of a modified strong cation exchange material named MEX and its application in 2D-MEX × C18 system to separate peptides from scorpion venom.

PubMed

Chen, Bo; Xu, Junyan; Fu, Qing; Dong, Xuefang; Guo, Zhimou; Jin, Yu; Liang, Xinmiao

2015-07-07

Peptides from scorpion venom represent one of the most promising drug sources for drug discovery for some specific diseases. Current challenges in their separation include high complexity, high homologies and the huge range of peptides. In this paper, a modified strong cation exchange material, named MEX, was utilised for the two-dimensional separation of peptides from complex scorpion venom. The silica-based MEX column was bonded with two functional groups; benzenesulfonic acid and cyanopropyl. To better understand its separation mechanisms, seven standard peptides with different properties were employed in an evaluation study, the results of which showed that two interactions were involved in the MEX column: electrostatic interactions based on benzenesulfonic acid groups dominated the separation of peptides; weak hydrophobic interactions introduced by cyanopropyl groups increased the column's selectivity for peptides with the same charge. This characteristic allowed the MEX column to overcome some of the drawbacks of traditional strong cation exchange (SCX) columns. Furthermore, the study showed the great effects of the acetonitrile (ACN) content, the sodium perchlorate (NaClO4) concentration and the buffer pH in the mobile phase on the peptides' retention and separation selectivity on the MEX column. Subsequently, the MEX column was combined with a C18 column to establish an off-line 2D-MEX × C18 system to separate peptides from scorpion Buthus martensi Karsch (BmK) venom. Due to complementary separation mechanisms in each dimension, a high orthogonality of 47.62% was achieved. Moreover, a good loading capacity, excellent stability and repeatability were exhibited by the MEX column, which are beneficial for its use in future preparation experiments. Therefore, the MEX column could be an alternative to the traditional SCX columns for the separation of peptides from scorpion venom.

HPLC enantioseparation of racemic bupropion, baclofen and etodolac: modification of conventional ligand exchange approach by pre-column formation of chiral ligand exchange complexes.

PubMed

Singh, Manisha; Bhushan, Ravi

2016-11-01

Separation of racemic mixture of (RS)-bupropion, (RS)-baclofen and (RS)-etodolac, commonly marketed racemic drugs, has been achieved by modifying the conventional ligand exchange approach. The Cu(II) complexes were first prepared with a few l-amino acids, namely, l-proline, l-histidine, l-phenylalanine and l-tryptophan, and to these was introduced a mixture of the enantiomer pair of (RS)-bupropion, or (RS)-baclofen or (RS)-etodolac. As a result, formation of a pair of diastereomeric complexes occurred by 'chiral ligand exchange' via the competition between the chelating l-amino acid and each of the two enantiomers from a given pair. The diastereomeric mixture formed in the pre-column process was loaded onto HPLC column. Thus, both the phases during chromatographic separation process were achiral (i.e. neither the stationary phase had any chiral structural feature of its own nor did the mobile phase have any chiral additive). Separation of diastereomers was successful using a C 18 column and a binary mixture of MeCN and TEAP buffer of pH 4.0 (60:40, v/v) as mobile phase at a flow rate of 1 mL/min and UV detection at 230 nm for (RS)-Bup, 220 nm for (RS)-Bac and 223 nm for (RS)-Etd. Baseline separation of the two enantiomers was obtained with a resolution of 6.63 in <15 min. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

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.

Method for the chemical separation of GE-68 from its daughter Ga-68

DOEpatents

Fitzsimmons, Jonathan M.; Atcher, Robert W.

2010-06-01

The present invention is directed to a generator apparatus for separating a daughter gallium-68 radioisotope substantially free of impurities from a parent gernanium-68 radioisotope, including a first resin-containing column containing parent gernanium-68 radioisotope and daughter gallium-68 radioisotope, a source of first eluent connected to said first resin-containing column for separating daughter gallium-68 radioisotope from the first resin-containing column, said first eluent including citrate whereby the separated gallium is in the form of gallium citrate, a mixing space connected to said first resin-containing column for admixing a source of hydrochloric acid with said separated gallium citrate whereby gallium citrate is converted to gallium tetrachloride, a second resin-containing column for retention of gallium-68 tetrachloride, and, a source of second eluent connected to said second resin-containing column for eluting the daughter gallium-68 radioisotope from said second resin-containing column.

Improvement in HPLC separation of acetic acid and levulinic acid in the profiling of biomass hydrolysate.

PubMed

Xie, Rui; Tu, Maobing; Wu, Yonnie; Adhikari, Sushil

2011-04-01

5-Hydroxymethylfurfural (HMF) and furfural could be separated by the Aminex HPX-87H column chromatography, however, the separation and quantification of acetic acid and levulinic acid in biomass hydrolysate have been difficult with this method. In present study, the HPLC separation of acetic acid and levulinic acid on Aminex HPX-87H column has been investigated by varying column temperature, flow rate, and sulfuric acid content in the mobile phase. The column temperature was found critical in resolving acetic acid and levulinic acid. The resolution for two acids increased dramatically from 0.42 to 1.86 when the column temperature was lowered from 60 to 30 °C. So did the capacity factors for levulinic acid that was increased from 1.20 to 1.44 as the column temperature dropped. The optimum column temperature for the separation was found at 45 °C. Variation in flow rate and sulfuric acid concentration improved not as much as the column temperature did. Published by Elsevier Ltd.

Sequential elution process

DOEpatents

Kingsley, I.S.

1987-01-06

A process and apparatus are disclosed for the separation of complex mixtures of carbonaceous material by sequential elution with successively stronger solvents. In the process, a column containing glass beads is maintained in a fluidized state by a rapidly flowing stream of a weak solvent, and the sample is injected into this flowing stream such that a portion of the sample is dissolved therein and the remainder of the sample is precipitated therein and collected as a uniform deposit on the glass beads. Successively stronger solvents are then passed through the column to sequentially elute less soluble materials. 1 fig.

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.

METHOD OF AND APPARATUS FOR WITHDRAWING LIGHT ISOTOPIC PRODUCT FROM A LIQUID THERMAL DIFFUSION PLANT

DOEpatents

Dole, M.

1959-09-22

An improved process and apparatus are described for removing enriched product from the columns of a thermal diffusion plant for separation of isotopes. In the removal cycle, light product at the top cf the diffusion columns is circulated through the column tops and a shipping cylinder connected thereto unttl the concertation of enriched product in the cylinder reaches the desired point. During the removal, circulation through the bottoms is blocked bv freezing. in the diffusion cycle, the bottom portion is unfrozen, fresh feed is distributed to the bottoms of the columns, ard heavy product is withdrawn from the bottoms, while the tops of the columns are blocked by freezing.

Green Chromatographic Separation of Coumarin and Vanillins Using Subcritical Water as the Mobile Phase.

PubMed

Kayan, Berkant; Akay, Sema; Yang, Yu

2016-08-01

Pure water was used as the eluent for separation of coumarin, vanillin and ethyl vanillin at temperatures ranging from 100 to 200°C using a homemade subcritical water chromatography (SBWC) system. Chromatographic separations were performed on five commercial columns including XTerra MS C18, XBridge C18, Zorbax RRHD Eclipse Plus, Zorbax SB-Phenyl and Zorbax SB-C18 columns. The retention time of all three solutes decreased with increasing water temperature. The shortest retention time among all acceptable separations, less than 4 min, was achieved on the Zorbax SB-C18 column at 200°C. While separations on the XTerra MS C18 column resulted in fronting peaks and a degradation peak from ethyl vanillin on the Zorbax RRHD Eclipse Plus column was observed, all three other columns yielded reasonable separations under SBWC conditions. In addition to separation of the standard test mixture, separation of coumarin contained in a skincare cream sample was also carried out using SBWC. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

PubMed

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

2006-04-01

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

Miniaturized protein separation using a liquid chromatography column on a flexible substrate

NASA Astrophysics Data System (ADS)

Yang, Yongmo; Chae, Junseok

2008-12-01

We report a prototype protein separator that successfully miniaturizes existing technology for potential use in biocompatible health monitoring implants. The prototype is a liquid chromatography (LC) column (LC mini-column) fabricated on an inexpensive, flexible, biocompatible polydimethylsiloxane (PDMS) enclosure. The LC mini-column separates a mixture of proteins using size exclusion chromatography (SEC) with polydivinylbenzene beads (5-20 µm in diameter with 10 nm pore size). The LC mini-column is smaller than any commercially available LC column by a factor of ~11 000 and successfully separates denatured and native protein mixtures at ~71 psi of the applied fluidic pressure. Separated proteins are analyzed using NuPAGE-gel electrophoresis, high-performance liquid chromatography (HPLC) and an automated electrophoresis system. Quantitative HPLC results demonstrate successful separation based on intensity change: within 12 min, the intensity between large and small protein peaks changed by a factor of ~20. In further evaluation using the automated electrophoresis system, the plate height of the LC mini-column is between 36 µm and 100 µm. The prototype LC mini-column shows the potential for real-time health monitoring in applications that require inexpensive, flexible implant technology that can function effectively under non-laboratory conditions.

Investigation of transient cavitating flow in viscoelastic pipes

NASA Astrophysics Data System (ADS)

Keramat, A.; Tijsseling, A. S.; Ahmadi, A.

2010-08-01

A study on water hammer in viscoelastic pipes when the fluid pressure drops to liquid vapour pressure is performed. Two important concepts including column separation and the effects of retarded strains in the pipe wall on the fluid response have been investigated separately in recent works, but there is some curiosity as to how the results for pressure and discharge are when column separation occurs in a viscoelastic pipe. For pipes made of plastic such as polyethylene (PE) and polyvinyl chloride (PVC), viscoelasticity is a crucial mechanical property which changes the hydraulic and structural transient responses. Based on previous developments in the analysis of water hammer, a model which is capable of analysing column separation in viscoelastic pipes is presented and used for solving the selected case studies. For the column-separation modelling the Discrete Vapour Cavity Model (DVCM) is utilised and the viscoelasticity property of the pipe wall is modelled by Kelvin-Voigt elements. The effects of viscoelasticity play an important role in the column separation phenomenon because it changes the water hammer fundamental frequency and so affects the time of opening or collapse of the cavities. Verification of the implemented computer code is performed for the effects of viscoelasticity and column separation - separately and simultaneously - using experimental results from the literature. In the provided examples the focus is placed on the simultaneous effect of viscoelasticity and column separation on the hydraulic transient response. The final conclusions drawn are that if rectangular grids are utilised the DVCM gives acceptable predictions of the phenomenon and that the pipe wall material's retarded behaviour strongly dampens the pressure spikes caused by column separation.

Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

NASA Technical Reports Server (NTRS)

Huz, Kateryna

2014-01-01

RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better detection via good peak separation with a longer run time is a better asset than moderate peak separation with a shorter run time. Even given that RESOLVE is highly interested in water and that mission timeline is of significant importance given the short seven-to-ten-day mission timeline, worse detection with an 8m column may lead to overlooking other substances existing on the moon that could advance planetary science. Thus, I recommend the 20m column. However, if mission timeline and water separation are deemed the highest priority, the 8m column should be selected due to its ability to separate water within a shorter run time than the 20m column.

Determination of pesticide residues in food with a 6% cyanopropylphenyl capillary column.

PubMed

Daft, J L

1989-02-01

A small-diameter 6% cyanopropylphenyl column is studied for its suitability for determining pesticides in food. Repeatability and linearity are satisfactory, and the column is capable of separating residue combinations that are known not to separate on methyl silicone columns. At 150 degrees C or 130 degrees C, the column satisfactorily separates five by-products of tecnazene, a growth regulator and sprout suppressant found in potatoes, and four by-products of quintozene, a soil and seed fungicide found in peanut products.

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.

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

PubMed

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

2016-03-01

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

A modified approach for isolation of essential oil from fruit of Amorpha fruticosa Linn using microwave-assisted hydrodistillation concatenated liquid-liquid extraction.

PubMed

Chen, Fengli; Jia, Jia; Zhang, Qiang; Gu, Huiyan; Yang, Lei

2017-11-17

In this work, a modified technique was developed to separate essential oil from the fruit of Amorpha fruticosa using microwave-assisted hydrodistillation concatenated liquid-liquid extraction (MHD-LLE). The new apparatus consists of two series-wound separation columns for separating essential oil, one is the conventional oil-water separation column, and the other is the extraction column of components from hydrosol using an organic solvent. Therefore, the apparatus can simultaneously collect the essential oil separated on the top of hydrosol and the components extracted from hydrosol using an organic solvent. Based on the yield of essential oil in the first and second separation columns, the effects of parameters were investigated by single factor experiments and Box-Behnken design. Under the optimum conditions (2mL ethyl ether as the extraction solvent in the second separation column, 12mL/g liquid-solid ratio, 4.0min homogenate time, 35min microwave irradiation time and 540W microwave irradiation power), satisfactory yields for the essential oil in the first separation column (10.31±0.33g/kg) and second separation column (0.82±0.03g/kg) were obtained. Compared with traditional methods, the developed method gave a higher yield of essential oil in a shorter time. In addition, GC-MS analysis of the essential oil indicated significant differences of the relative contents of individual volatile components in the essential oils obtained in the two separation columns. Therefore, the MHD-LLE technique developed here is a good alternative for the isolation of essential oil from A. fruticosa fruit as well as other herbs. Copyright © 2017 Elsevier B.V. All rights reserved.

Observation and explanation of two-dimensional interconversion of oximes with multiple heart-cutting using comprehensive multidimensional gas chromatography.

PubMed

Kulsing, Chadin; Nolvachai, Yada; Wong, Yong Foo; Glouzman, Melissa I; Marriott, Philip J

2018-04-20

Real-time interconversion processes produce unconventional peak broadening in gas chromatography (GC), and can be used to generate kinetic and thermodynamic data. In this study, an unusual separation situation in comprehensive two dimensional GC where two dimensional interconversion (i.e. a raised plateau in both first and second dimension, 1 D and 2 D) was observed in analysis of oxime isomers. This resulted in a characteristic and unusual rectangular peak shape in the two dimensional result. A related theoretical approach was introduced to explain the peak shape supported by simulation results which can be varied depending on concentration profiles and kinetics of the process. The simulated results were supported by experimental results obtained by a comprehensive heart-cut multidimensional GC (H/C MDGC) approach which was developed to clearly investigate isomerisation of E/Z oxime molecules in both 1 D and 2 D separations under different isothermal conditions. The carrier gas flow and oven temperature were selected according to initial results for 1D interconversion on a poly(ethyleneglycol) stationary phase, which was further used in both 1 D and 2 D separations to result in broad zones of oxime interconversion in both dimensions. The method involved repetitive injections of oxime sample, then sampling contiguous fractions of sample into a long 2 D column which is intended to promote considerable interconversion. Comprehensiveness arises from the fact that the whole sample is sampled from the 1 D to the 2 D column, with the long 2 D column replacing the short 2 D column used in classical comprehensive two-dimensional gas chromatography, where the latter will not promote sufficient interconversion. Data processing and presentation permits a 'rectangular' distribution corresponding to the separated compounds, characteristic of this experiment. Copyright © 2018 Elsevier B.V. All rights reserved.

Sugar, acid and furfural quantification in a sulphite pulp mill: Feedstock, product and hydrolysate analysis by HPLC/RID.

PubMed

Llano, Tamara; Quijorna, Natalia; Andrés, Ana; Coz, Alberto

2017-09-01

Waste from pulp and paper mills consist of sugar-rich fractions comprising hemicellulose derivatives and cellulose by-products. A complete characterisation of the waste streams is necessary to study the possibilities of an existing mill. In this work, four chromatographic methods have been developed to obtain the most suitable chromatographic method conditions for measuring woody feedstocks, lignocellulosic hydrolysates and cellulose pulp in sulphite pulping processes. The analysis of major and minor monosaccharides, aliphatic carboxylic acids and furfurals has been optimised. An important drawback of the spent liquors generated after sulphite pulping is their acidic nature, high viscosity and adhesive properties that interfere in the column lifetime. This work recommends both a CHO-782Pb column for the sugar analysis and an SH-1011 resin-based cross-linked gel column to separate low-molecular-weight chain acids, alcohols and furfurals. Such columns resulted in a good separation with long lifetime, wide pH operating range and low fouling issues.

METHOD OF OPERATING A HEAVY WATER MODERATED REACTOR

DOEpatents

Vernon, H.C.

1962-08-14

A method of removing fission products from the heavy water used in a slurry type nuclear reactor is described. According to the process the slurry is steam distilled with carbon tetrachloride so that at least a part of the heavy water and carbon tetrachloride are vaporized; the heavy water and carbon tetrachloride are separated; the carbon tetrachloride is returned to the steam distillation column at different points in the column to aid in depositing the slurry particles at the bottom of the column; and the heavy water portion of the condensate is purified. (AEC)

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.

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.

Chromatographic hydrogen isotope separation

DOEpatents

Aldridge, Frederick T.

1981-01-01

Intermetallic compounds with the CaCu.sub.5 type of crystal structure, particularly LaNiCo.sub.4 and CaNi.sub.5, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation colum. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale mutli-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen can produce large quantities of heavy water at an effective cost for use in heavy water reactors.

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.

Programmable selectivity for GC with series-coupled columns using pulsed heating of the second column.

PubMed

Whiting, Joshua; Sacks, Richard

2003-05-15

A series-coupled ensemble of a nonpolar dimethyl polysiloxane column and a polar trifluoropropylmethyl polysiloxane column with independent at-column heating is used to obtain pulsed heating of the second column. For mixture component bands that are separated by the first column but coelute from the column ensemble, a temperature pulse is initiated after the first of the two components has crossed the column junction point and is in the second column, while the other component is still in the first column. This accelerates the band for the first component. If the second column cools sufficiently prior to the second component band crossing the junction, the second band experiences less acceleration, and increased separation is observed for the corresponding peaks in the ensemble chromatogram. High-speed at-column heating is obtained by wrapping the fused-silica capillary column with resistance heater wire and sensor wire. Rapid heating for a temperature pulse is obtained with a short-duration linear heating ramp of 1000 degrees C/min. During a pulse, the second-column temperature increases by 20-100 degrees C in a few seconds. Using a cold gas environment, cooling to a quiescent temperature of 30 degrees C can be obtained in approximately 25 s. The effects of temperature pulse initiation time and amplitude on ensemble peak separation and resolution are described. A series of appropriately timed temperature pulses is used to separate three coeluting pairs of components in a 13-component mixture.

[Advances of the coatings used in columns for capillary electrophoresis and in nanochannels of chips].

PubMed

Liu, Chunye; Chen, Jierong

2005-01-01

An overview is provided on the advancement and development of coating preparation methodology and materials used in capillaries and channels in microfluidic chip. Discussion is also given on the effects of coatings in the resolutions of separation and the reproducibility of separations. Dynamic coatings and linked coatings, classified as homo-polymers, copolymers and heterocyclic compounds, are further discussed, and so are the methods for the preparation of the coatings by cross-linked reaction, sol-gel process, photomodification and chemical deposition, etc. The discussion will be useful for the optimization of capillary columns that are used in capillary electrophoresis and nanochannels of chip.

Evaluation of center-cut separations applying simulated moving bed chromatography with 8 zones.

PubMed

Santos da Silva, Francisco Vitor; Seidel-Morgenstern, Andreas

2016-07-22

Different multi-column options to perform continuous chromatographic separations of ternary mixtures have been proposed in order to overcome limitations of batch chromatography. One attractive option is given by simulated moving bed chromatography (SMB) with 8 zones, a process that offers uninterrupted production, and, potentially, improved economy. As in other established ternary separation processes, the separation sequence is crucial for the performance of the process. This problem is addressed here by computing and comparing optimal performances of the two possibilities assuming linear adsorption isotherms. The conclusions are presented in a decision tree which can be used to guide the selection of system configuration and operation. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2006-01-20

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

Extraction chromatographic separation of Am(III) and Eu(III) by TPEN-immobilized gel

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

Takeshita, K.; Ogata, T.; Oaki, H.

2013-07-01

A TPEN derivative with 4 vinyl groups, N,N,N',N' -tetrakis-(4-propenyloxy-2-pyridylmethyl)ethylenediamine (TPPEN) was synthesized for the separation of trivalent minor actinides (Am(III)) and lanthanides (Eu(III)). A co-polymer gel with TPPEN and N-isopropylacrylamide (NIPA) showed a high separation factor of Am(III) over Eu(III) (SF[Am/Eu]), which was evaluated to be 26 at pH=5. Thin film of NIPA-TPPEN gel (average thickness: 2-40 nm) was immobilized on the pore surface in porous silica particles (particle diameter : 50 μm, average pore diameter : 50 and 300 nm) and a chromatographic column (diameter: 6 mm, height: 11 mm) packed with the gel-coated particles was prepared. A smallmore » amount of weakly acidic solution (pH=4) containing Am(III) and Eu(III) was supplied in the column and the elution tests of Am(III) and Eu(III) were carried out. Eu(III) was recovered separately by a weakly acidic eluent (pH=4) at 313 K and Am(III) by a highly acidic eluent (pH=2) at 298 K. These results suggest that the contentious separation of minor actinides and lanthanides is attainable by a new extraction chromatographic process with two columns adjusted to 298 K and 313 K. (authors)« less

Chiral ligand-exchange high-performance liquid chromatography with copper (II)-L-phenylalanine complexes for separation of 3,4-dimethoxy-α-methylphenylalanine racemes.

PubMed

Jia, Dong-Xu; Ai, Zheng-Gui; Xue, Ya-Ping; Zheng, Yu-Guo

2014-11-01

L-3, 4-dimethoxy-α-methylphenylalanine (L-DMMD) is an important intermediate for the synthesis of 3-hydroxy-α-methyl-L-tyrosine (L-methyldopa). This paper describes an efficient, accurate, and low-priced method of high-performance liquid chromatography (HPLC) using chiral mobile phase and conventional C18 column to separate L-DMMD from its enantiomers. The effects of ligands, copper salts, organic modifiers, pHs of mobile phase, and temperatures on the retention factors (k') and selectivity (α) were evaluated to achieve optimal separation performance. Then, thermal analysis of the optimal separation conditions was investigated as well. It was confirmed that the optimal mobile phase was composed of 20 % (v/v) methanol, 8 mM L-phenylalanine (L-Phe), and 4 mM cupric sulfate in water of pH 3.2, and the column temperature was set at 20 °C. Baseline separation of two enantiomers could be obtained through the conventional C18 column with a resolution (R) of 3.18 in less than 18 min. Thermodynamic data (∆∆H and ∆∆S) obtained by Van't Hoff plots revealed the chiral separation was an enthalpy-controlled process. To the best of our knowledge, this is the first report regarding the enantioseparation of DMMD by chiral ligand-exchange HPLC.

Multi-mode application of graphene quantum dots bonded silica stationary phase for high performance liquid chromatography.

PubMed

Wu, Qi; Sun, Yaming; Zhang, Xiaoli; Zhang, Xia; Dong, Shuqing; Qiu, Hongdeng; Wang, Litao; Zhao, Liang

2017-04-07

Graphene quantum dots (GQDs), which possess hydrophobic, hydrophilic, π-π stacking and hydrogen bonding properties, have great prospect in HPLC. In this study, a novel GQDs bonded silica stationary phase was prepared and applied in multiple separation modes including normal phase, reversed phase and hydrophilic chromatography mode. Alkaloids, nucleosides and nucleobases were chosen as test compounds to evaluate the separation performance of this column in hydrophilic chromatographic mode. The tested polar compounds achieved baseline separation and the resolutions reached 2.32, 4.62, 7.79, 1.68 for thymidine, uridine, adenosine, cytidine and guanosine. This new column showed satisfactory chromatographic performance for anilines, phenols and polycyclic aromatic hydrocarbons in normal and reversed phase mode. Five anilines were completely separated within 10min under the condition of mobile phase containing only 10% methanol. The effect of water content, buffer concentration and pH on chromatographic separation was further investigated, founding that this new stationary phase showed a complex retention mechanism of partitioning, adsorption and electrostatic interaction in hydrophilic chromatography mode, and the multiple retention interactions such as π-π stacking and π-π electron-donor-acceptor interaction played an important role during the separation process. This GQDs bonded column, which allows us to adjust appropriate chromatography mode according to the properties of analytes, has possibility in actual application after further research. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation and characterization of polycyclic aromatic hydrocarbons and alkylphenols in coal derived solvents

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

Hurtubise, R.J.; Allen, T.W.; Hussain, A.

1981-03-29

Dry-column chromatography with an aluminum oxide stationary phase and a n-hexane-ether (19:1) mobile phase was used to separate polycyclic aromatic hydrocarbons (PAH) by ring size. Prior to the dry-column chromatography step, the coal derived solvents were added to an acid treated silica gel column and eluted with chloroform. This step removed pyridine-type nitrogen heterocycles. After separation of the individual ring fractions, the fractions were further separated by either thin layer chromatography (TLC) or high performance liquid chromatography (HPLC). If TLC was used, then after separation fluorescence profiles of each PAH ring fraction distributed on 30%-acetylated cellulose chromatoplates were obtained withmore » a spectrodensitometer. Measurement of fluorescence peak heights gave an approximate measure of the amount of the 3-, 4-, 5-, and 6- ring PAH. For HPLC separation, the 3- and 4- ring PAH fractions obtained from the dry-column chromatography step were separated with a ..mu..-Bondapak C/sub 18/ column and methanol:water (65:35) mobile phase. The HPLC separated PAH were characterized by chromatographic correlation factors and corrected fluorescence excitation spectra. Alkylphenols were identified in coal recycle solvent sample following separation by HPLC.« less

The Use of Cryogenically Cooled 5A Molecular Sieves for Large Volume Reduction of Tritiated Hydrogen Gas

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

Antoniazzi, A.B.; Bartoszek, F.E.; Sherlock, A.M.

2006-07-01

A commercial hydrogen isotope separation system based on gas chromatography (AGC-ISS) has been built. The system operates in two modes: stripping and volume reduction. The purpose of the stripping mode is to reduce a large volume of tritiated hydrogen gas to a small volume of tritium rich hydrogen gas. The results here illustrate the effectiveness of the AGC-ISS in the stripping and volume reduction phases. Column readiness for hydrogen isotope separation is confirmed by room temperature air separation tests. Production runs were initially carried out using natural levels of deuterium (110-160 ppm) in high purity hydrogen. After completion of themore » deuterium/hydrogen runs the system began operations with tritiated hydrogen. The paper presents details of the AGC-ISS design and results of tritium tests. The heart of the AGC-ISS consists of two packed columns (9 m long, 3.8 cm OD) containing 5A molecular sieve material of 40/60 mesh size. Each column has 5 individually controlled heaters along the length of the column and is coiled around an inverted inner dewar. The coiled column and inner dewar are both contained within an outer dewar. In this arrangement liquid nitrogen, used to cryogenically cool the columns, flows into and out off the annular space defined by the two dewars, allowing for alternate heating and cooling cycles. Tritiated hydrogen feed is injected in batch quantities. The batch size is variable with the maximum quantity restricted by the tritium concentration in the exhausted hydrogen. The stripping operations can be carried out in full automated mode or in full manual mode. The average cycle time between injections is about 75 minutes. To date, the maximum throughput achieved is 10.5 m{sup 3}/day. A total of 37.8 m{sup 3} of tritiated hydrogen has been processed during commissioning. The system has demonstrated that venting of >99.95% of the feed gas is possible while retaining 99.98% of the tritium. At a maximum tritium concentration of {approx}7 GBq/m{sup 3} (190 mCi/m{sup 3}), processing tritiated hydrogen gas at a rate of 8.1 m{sup 3} (NTP)/day results in an average tritium concentration in the process effluent line of 1.4 MBq/m{sup 3} (37 {mu}Ci/m{sup 3}). The average process exhaust flow, split between helium and hydrogen, is 10.6 litre/min. Product from the stripping phase is stored on a 5 kg depleted uranium bed. A 250 g depleted uranium bed is available for storage of enriched product. Several, ionization type, tritium sensors are located throughout the process to control emissions, control valve switching, and monitor evolution of tritiated species from the columns. (authors)« less

Liquid-liquid phase separation causes high turbidity and pressure during low pH elution process in Protein A chromatography.

PubMed

Luo, Haibin; Lee, Nacole; Wang, Xiangyang; Li, Yuling; Schmelzer, Albert; Hunter, Alan K; Pabst, Timothy; Wang, William K

2017-03-10

Turbid elution pools and high column back pressure are common during elution of monoclonal antibodies (mAbs) by acidic pH in Protein A chromatography. This phenomenon has been historically attributed to acid-induced precipitation of incorrectly folded or pH-sensitive mAbs and host cell proteins (HCPs). In this work, we propose a new mechanism that may account for some observations of elution turbidity in Protein A chromatography. We report several examples of turbidity and high column back pressure occurring transiently under a short course of neutral conditions during Protein A elution. A systematic study of three mAbs displaying this behavior revealed phase separation characterized by liquid drops under certain conditions including neutral pH, low ionic strength, and high protein concentration. These liquid droplets caused solution turbidity and exhibited extremely high viscosity, resulting in high column back pressure. We found out that the droplets were formed through liquid-liquid phase separation (LLPS) as a result of protein self-association. We also found multiple factors, including pH, temperature, ionic strength, and protein concentration can affect LLPS behaviors. Careful selection of process parameters during protein A elution, including temperature, flow rate, buffer, and salt can inhibit formation of a dense liquid phase, reducing both turbidity (by 90%) and column back pressure (below 20 pounds per square inch). These findings provide both mechanistic insight and practical mitigation strategies for Protein A chromatography induced LLPS. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Targeted Therapies for Myeloma and Metastatic Bone Cancers

DTIC Science & Technology

2007-02-01

increased efficacy in the targeted microenvironment, and the ultimate opportunity to reverse catastrophic disease processes . Furthermore, targeted...concentrate the resulting nanoparticles using centrifuge concentrator tubes and we have integrated this processing step into our nanoparticle...is unaffected by this slightly altered approach. Furthermore, this modified method avoids a lengthy column separation process that diminishes the

Identification of column edges of DNA fragments by using K-means clustering and mean algorithm on lane histograms of DNA agarose gel electrophoresis images

NASA Astrophysics Data System (ADS)

Turan, Muhammed K.; Sehirli, Eftal; Elen, Abdullah; Karas, Ismail R.

2015-07-01

Gel electrophoresis (GE) is one of the most used method to separate DNA, RNA, protein molecules according to size, weight and quantity parameters in many areas such as genetics, molecular biology, biochemistry, microbiology. The main way to separate each molecule is to find borders of each molecule fragment. This paper presents a software application that show columns edges of DNA fragments in 3 steps. In the first step the application obtains lane histograms of agarose gel electrophoresis images by doing projection based on x-axis. In the second step, it utilizes k-means clustering algorithm to classify point values of lane histogram such as left side values, right side values and undesired values. In the third step, column edges of DNA fragments is shown by using mean algorithm and mathematical processes to separate DNA fragments from the background in a fully automated way. In addition to this, the application presents locations of DNA fragments and how many DNA fragments exist on images captured by a scientific camera.

HPLC separation of triacylglycerol positional isomers on a polymeric ODS column.

PubMed

Kuroda, Ikuma; Nagai, Toshiharu; Mizobe, Hoyo; Yoshimura, Nobuhito; Gotoh, Naohiro; Wada, Shun

2008-07-01

A polymeric ODS column was applied to the resolution of triacylglycerol positional isomers (TAG-PI), i.e. 1,3-dioleoyl-2-palmitoyl-glycerol (OPO) and 1,2-dioleoyl-3-palmitoyl-rac-glycerol (OOP), with a recycle HPLC system. To investigate the ODS column species and the column temperatures for the resolution of a TAG-PI pair, a mixture of OPO and OOP was subjected to an HPLC system equipped with a non-endcapped polymeric, endcapped monomeric, endcapped intermediate, or non-endcapped monomeric ODS column at three different column temperatures (40, 25, or 10 degrees C). Only the non-endcapped polymeric ODS column achieved the separation of OPO and OOP, and the lowest column temperature (10 degrees C) showed the best resolution for them. The other pair of TAG-PI, a mixture of 1,3-dipalmitoyl-2-oleoyl-glycerol (POP) and 1,2-dipalmitoyl-3-oleoyl-rac-glycerol (PPO) was also subjected to the system equipped with a non-endcapped polymeric or monomeric ODS column at five different column temperatures (40, 32, 25, 17, and 10 degrees C). Thus, POP and PPO were also separated on only the non-endcapped polymeric ODS column at 25 degrees C. However, no clear peak appeared at 10 degrees C. These results would indicate that the polymeric ODS stationary phase has an ability to recognize the structural differences between TAG-PI pairs. Also, the column temperature is a very important factor for separating the TAG-PI pair, and the optimal temperature would relate to the solubility of TAG-PI in the mobile phase. Furthermore, the recycle HPLC system provided measurements for the separation and analysis of TAG-PI pairs.

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.

Mathematical analysis of frontal affinity chromatography in particle and membrane configurations.

PubMed

Tejeda-Mansir, A; Montesinos, R M; Guzmán, R

2001-10-30

The scaleup and optimization of large-scale affinity-chromatographic operations in the recovery, separation and purification of biochemical components is of major industrial importance. The development of mathematical models to describe affinity-chromatographic processes, and the use of these models in computer programs to predict column performance is an engineering approach that can help to attain these bioprocess engineering tasks successfully. Most affinity-chromatographic separations are operated in the frontal mode, using fixed-bed columns. Purely diffusive and perfusion particles and membrane-based affinity chromatography are among the main commercially available technologies for these separations. For a particular application, a basic understanding of the main similarities and differences between particle and membrane frontal affinity chromatography and how these characteristics are reflected in the transport models is of fundamental relevance. This review presents the basic theoretical considerations used in the development of particle and membrane affinity chromatography models that can be applied in the design and operation of large-scale affinity separations in fixed-bed columns. A transport model for column affinity chromatography that considers column dispersion, particle internal convection, external film resistance, finite kinetic rate, plus macropore and micropore resistances is analyzed as a framework for exploring further the mathematical analysis. Such models provide a general realistic description of almost all practical systems. Specific mathematical models that take into account geometric considerations and transport effects have been developed for both particle and membrane affinity chromatography systems. Some of the most common simplified models, based on linear driving-force (LDF) and equilibrium assumptions, are emphasized. Analytical solutions of the corresponding simplified dimensionless affinity models are presented. Particular methods for estimating the parameters that characterize the mass-transfer and adsorption mechanisms in affinity systems are described.

COLUMBIC OXIDE ADSORPTION PROCESS FOR SEPARATING URANIUM AND PLUTONIUM IONS

DOEpatents

Beaton, R.H.

1959-07-14

A process is described for separating plutonium ions from a solution of neutron irradiated uranium in which columbic oxide is used as an adsorbert. According to the invention the plutonium ion is selectively adsorbed by Passing a solution containing the plutonium in a valence state not higher than 4 through a porous bed or column of granules of hydrated columbic oxide. The adsorbed plutonium is then desorbed by elution with 3 N nitric acid.

Enantiomeric separation of type I and type II pyrethroid insecticides with different chiral stationary phases by reversed-phase high-performance liquid chromatography.

PubMed

Zhang, Ping; Yu, Qian; He, Xiulong; Qian, Kun; Xiao, Wei; Xu, Zhifeng; Li, Tian; He, Lin

2018-04-01

The enantiomeric separation of type I (bifenthrin, BF) and type II (lambda-cyhalothrin, LCT) pyrethroid insecticides on Lux Cellulose-1, Lux Cellulose-3, and Chiralpak IC chiral columns was investigated by reversed-phase high-performance liquid chromatography. Methanol/water or acetonitrile/water was used as mobile phase at a flow rate of 0.8 mL/min. The effects of chiral stationary phase, mobile phase composition, column temperature, and thermodynamic parameters on enantiomer separation were carefully studied. Bifenthrin got a partial separation on Lux Cellulose-1 column and baseline separation on Lux Cellulose-3 column, while LCT enantiomers could be completely separated on both Lux Cellulose-1 and Lux Cellulose-3 columns. Chiralpak IC provided no separation ability for both BF and LCT. Retention factor (k) and selectivity factor (α) decreased with the column temperature increasing from 10°C to 40°C for both BF and LCT enantiomers. Thermodynamic parameters including ∆H and ∆S were also calculated, and the maximum R s were not always obtained at lowest temperature. Furthermore, the quantitative analysis methods for BF and LCT enantiomers in soil and water were also established. Such results provide a new approach for pyrethroid separation under reversed-phase condition and contribute to environmental risk assessment of pyrethroids at enantiomer level. © 2017 Wiley Periodicals, Inc.

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

Palmieri, M.D.; Fritz, J.S.

Metal ions are determined by adding N-methylfurohydroxamic acid to an aqueous sample and then separating the metal chelates by direct injection onto a liquid chromatographic column. Separations on a C/sub 8/ silica column and a polystyrene-divinylbenzene column are compared, with better separations seen on the polymeric column. The complexes formed at low pH values are cationic and are separated by an ion pairing mechanism. Retention times and selectivity of the metal complexes can be varied by changing the pH. Several metal ions can be separated and quantified; separation conditions, linear calibration curve ranges, and detection limits are presented for Zr(IV),more » Hf(IV), Fe(III), Nb(V), Al(III), and Sb(III). Interferences due to the presence of other ions in solution are investigated. Finally, an antiperspirant sample is analyzed for zirconium by high-performance liquid chromatography.« less

Antibody-immobilized column for quick cell separation based on cell rolling.

PubMed

Mahara, Atsushi; Yamaoka, Tetsuji

2010-01-01

Cell separation using methodological standards that ensure high purity is a very important step in cell transplantation for regenerative medicine and for stem cell research. A separation protocol using magnetic beads has been widely used for cell separation to isolate negative and positive cells. However, not only the surface marker pattern, e.g., negative or positive, but also the density of a cell depends on its developmental stage and differentiation ability. Rapid and label-free separation procedures based on surface marker density are the focus of our interest. In this study, we have successfully developed an antiCD34 antibody-immobilized cell-rolling column, that can separate cells depending on the CD34 density of the cell surfaces. Various conditions for the cell-rolling column were optimized including graft copolymerization, and adjustment of the column tilt angle, and medium flow rate. Using CD34-positive and -negative cell lines, the cell separation potential of the column was established. We observed a difference in the rolling velocities between CD34-positive and CD34-negative cells on antibody-immobilized microfluidic device. Cell separation was achieved by tilting the surface 20 degrees and the increasing medium flow. Surface marker characteristics of the isolated cells in each fraction were analyzed using a cell-sorting system, and it was found that populations containing high density of CD34 were eluted in the delayed fractions. These results demonstrate that cells with a given surface marker density can be continuously separated using the cell rolling column.

Developing Inquiry-Based Labs Using Micro-Column Chromatography

ERIC Educational Resources Information Center

Barden-Gabbei, Laura M.; Moffitt, Deborah L.

2006-01-01

Chromatography is a process by which mixtures can be separated or substances can be purified. Biological and chemical laboratories use many different types of chromatographic processes. For example, the pharmaceutical industry uses chromatographic techniques to purify drugs, medical labs use them to identify blood components such as cholesterol,…

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

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.

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.

Branched-chain dicationic ionic liquids for fatty acid methyl ester assessment by gas chromatography.

PubMed

Talebi, Mohsen; Patil, Rahul A; Sidisky, Leonard M; Berthod, Alain; Armstrong, Daniel W

2017-12-06

Twelve bis- or dicationic ionic liquids (ILs) including eight based on imidazolium, a single one based on phosphonium, and three based on pyrrolidinium cationic units were prepared with the bis(trifluoromethyl sulfonyl) imide anion. The two identical cationic moieties were attached by different alkyl spacers having three or five carbons and differing alkyl substituents attached to the spacer. The SLB-IL111 column, as the most polar commercial stationary phase known, was included in the study for comparison. Isothermal separations of a rapeseed oil fatty acid methyl ester (FAME) sample were used to study and compare the 12 IL-based column performances and selectivities. The retention times of the most retained methyl esters of lignoceric (C24:0) and erucic (C22:1) acids were used to estimate the IL polarity. The phosphonium dicationic IL column was, by far, the least polar. Imidazolium-based dicationic IL columns were the most polar. Polarity and selectivity for the FAME separation were somewhat related. The separation of a 37-FAME standard mixture allowed the investigation of selectivity variations observed on the 12 IL-based columns under temperature gradients up to 230 °C. The remarkable selectivity of the IL-based columns is demonstrated by the detailed analysis of the cis/trans C18:1 isomers of a partially hydrogenated vegetable oil sample on 30-m columns, separations competing with that done following an "official method" performed on a 100-m column. Graphical abstract Separation of fatty acid methyl esters on a 30-m 3m 2 C 5 (mpy) 2 . 2NTf 2 branched-chain dicationic IL-based column. Branched chain dicationic ILs show great selectivity for separation of cis/trans, ω-3/ω-6, and detailed analysis of cis/trans fats.

Simple equations to simulate closed-loop recycling liquid-liquid chromatography: Ideal and non-ideal recycling models.

PubMed

Kostanyan, Artak E

2015-12-04

The ideal (the column outlet is directly connected to the column inlet) and non-ideal (includes the effects of extra-column dispersion) recycling equilibrium-cell models are used to simulate closed-loop recycling counter-current chromatography (CLR CCC). Simple chromatogram equations for the individual cycles and equations describing the transport and broadening of single peaks and complex chromatograms inside the recycling closed-loop column for ideal and non-ideal recycling models are presented. The extra-column dispersion is included in the theoretical analysis, by replacing the recycling system (connecting lines, pump and valving) by a cascade of Nec perfectly mixed cells. To evaluate extra-column contribution to band broadening, two limiting regimes of recycling are analyzed: plug-flow, Nec→∞, and maximum extra-column dispersion, Nec=1. Comparative analysis of ideal and non-ideal models has shown that when the volume of the recycling system is less than one percent of the column volume, the influence of the extra-column processes on the CLR CCC separation may be neglected. Copyright © 2015 Elsevier B.V. All rights reserved.

Separation of actinides using capillary extraction chromatography-inductively coupled plasma mass spectrometry.

PubMed

Peterson, Dominic S; Montoya, Velma M

2009-08-01

Trace levels of actinides have been separated on capillary extraction chromatography columns. Detection of the actinides was achieved using an inductively coupled plasma mass spectrometer, which was coupled with the extraction chromatography system. In this study, we compare 30-cm long, 4.6 mm i.d. columns to capillary columns (750 microm i.d.) with lengths from 30 cm up to 150 cm. The columns that were tested were packed with TRU resin. We were able to separate a mixture of five actinides ((232)Th, (238)U, (237)Np, (239)Pu, and (241)Am). This work has application to rapid bioassay as well as automated separations of actinide materials.

Separation of carbohydrates using hydrophilic interaction liquid chromatography.

PubMed

Fu, Qing; Liang, Tu; Li, Zhenyu; Xu, Xiaoyong; Ke, Yanxiong; Jin, Yu; Liang, Xinmiao

2013-09-20

A strategy was developed to rapidly evaluate chromatographic properties of hydrophilic interaction chromatography (HILIC) columns for separating carbohydrates. Seven HILIC columns (Silica, Diol, TSK Amide-80, XAmide, Click Maltose, Click β-CD, and Click TE-Cys columns) were evaluated by using three monosaccharide and seven disaccharides as probes. The influence of column temperature on the peak shape and tautomerization of carbohydrates, as well as column selectivity were investigated. The influence of surface charge property on the retention was also studied by using glucose, glucuronic acid, and glucosamine, which indicated that buffer salt concentration and pH value in mobile phase was necessary to control the ionic interactions between ionic carbohydrates and HILIC columns. According to evaluation results, the XAmide column was selected as an example to establish experimental schemes for separation of complex mixtures of oligosaccharide. Copyright © 2013 Elsevier Ltd. All rights reserved.

Development of High Precision Metal Micro-Electro-Mechanical-Systems Column for Portable Surface Acoustic Wave Gas Chromatograph

NASA Astrophysics Data System (ADS)

Iwaya, Takamitsu; Akao, Shingo; Sakamoto, Toshihiro; Tsuji, Toshihiro; Nakaso, Noritaka; Yamanaka, Kazushi

2012-07-01

In the field of environmental measurement and security, a portable gas chromatograph (GC) is required for the on-site analysis of multiple hazardous gases. Although the gas separation column has been downsized using micro-electro-mechanical-systems (MEMS) technology, an MEMS column made of silicon and glass still does not have sufficient robustness and a sufficiently low fabrication cost for a portable GC. In this study, we fabricated a robust and inexpensive high-precision metal MEMS column by combining diffusion-bonded etched stainless-steel plates with alignment evaluation using acoustic microscopy. The separation performance was evaluated using a desktop GC with a flame ionization detector and we achieved the high separation performance comparable to the best silicon MEMS column fabricated using a dynamic coating method. As an application, we fabricated a palm-size surface acoustic wave (SAW) GC combining this column with a ball SAW sensor and succeeded in separating and detecting a mixture of volatile organic compounds.

Practical comparison of LC columns packed with different superficially porous particles for the separation of small molecules and medium size natural products.

PubMed

Yang, Peilin; McCabe, Terry; Pursch, Matthias

2011-11-01

Commercial C(18) columns packed with superficially porous particles of different sizes and shell thicknesses (Ascentis Express, Kinetex, and Poroshell 120) or sub-2-μm totally porous particles (Acquity BEH) were systematically compared using a small molecule mixture and a complex natural product mixture as text probes. Significant efficiency loss was observed on 2.1-mm id columns even with a low dispersion ultra-high pressure liquid chromatography system. The Kinetex 4.6-mm id column packed with 2.6-μm particles exhibited the best overall efficiency for small molecule separations and the Poroshell 120 column showed better performance for mid-size natural product analytes. The Kinetex 2.1-mm id column packed with 1.7-μm particles did not deliver the expected performance and the possible reasons besides extra column effect have been proved to be frictional heating effect and poor column packing quality. Different column retentivities and selectivities have been observed on the four C(18) columns of different brands for the natural product separation. Column batch-to-batch variability that has been previously observed on the Ascentis Express column was also observed on the Kinetex and Poroshell 120 column. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Achieving high peak capacity production for gas chromatography and comprehensive two-dimensional gas chromatography by minimizing off-column peak broadening.

PubMed

Wilson, Ryan B; Siegler, W Christopher; Hoggard, Jamin C; Fitz, Brian D; Nadeau, Jeremy S; Synovec, Robert E

2011-05-27

By taking into consideration band broadening theory and using those results to select experimental conditions, and also by reducing the injection pulse width, peak capacity production (i.e., peak capacity per separation time) is substantially improved for one dimensional (1D-GC) and comprehensive two dimensional (GC×GC) gas chromatography. A theoretical framework for determining the optimal linear gas velocity (the linear gas velocity producing the minimum H), from experimental parameters provides an in-depth understanding of the potential for GC separations in the absence of extra-column band broadening. The extra-column band broadening is referred to herein as off-column band broadening since it is additional band broadening not due to the on-column separation processes. The theory provides the basis to experimentally evaluate and improve temperature programmed 1D-GC separations, but in order to do so with a commercial 1D-GC instrument platform, off-column band broadening from injection and detection needed to be significantly reduced. Specifically for injection, a resistively heated transfer line is coupled to a high-speed diaphragm valve to provide a suitable injection pulse width (referred to herein as modified injection). Additionally, flame ionization detection (FID) was modified to provide a data collection rate of 5kHz. The use of long, relatively narrow open tubular capillary columns and a 40°C/min programming rate were explored for 1D-GC, specifically a 40m, 180μm i.d. capillary column operated at or above the optimal average linear gas velocity. Injection using standard auto-injection with a 1:400 split resulted in an average peak width of ∼1.5s, hence a peak capacity production of 40peaks/min. In contrast, use of modified injection produced ∼500ms peak widths for 1D-GC, i.e., a peak capacity production of 120peaks/min (a 3-fold improvement over standard auto-injection). Implementation of modified injection resulted in retention time, peak width, peak height, and peak area average RSD%'s of 0.006, 0.8, 3.4, and 4.0%, respectively. Modified injection onto the first column of a GC×GC coupled with another high-speed valve injection onto the second column produced an instrument with high peak capacity production (500-800peaks/min), ∼5-fold to 8-fold higher than typically reported for GC×GC. Copyright © 2011 Elsevier B.V. All rights reserved.

New York State Department of Environmental Conservation PAMS monitoring system using a 3-column, double identification GC

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

Sierzenga, P.M.; Boynton, G.A.; Aho, B.J.

1996-12-31

New York State conducted its 1995 PAMS measurements for New York City in the Bronx borough (New York Botanical Gardens) using a Perkin-Elmer ATD-400 Thermal Desorbtion Unit with an 8000 Series Gas Chromatograph. Data was collected in New York City, transferred to Albany, and processed in the central office. The system was checked on a daily basis from Albany to verify operation. Quality assurance for the system was provided by collecting a one hour collocated canister sample every day with analysis performed in Albany using a GC-MS system. The normal configuration for the Perkin-Elmer system uses only two columns, amore » PLOT column to separate low weight hydrocarbons (C{sub 2}-C{sub 5}) and a BP-1 column to separate higher weight hydrocarbons (C{sub 6}-C{sub 10}). New York`s custom designed system uses a third RTX-5 column to provide a second identification and quantitation of most target hydrocarbons. Analysis of the 1995 data provides insight into the usefulness of the third column in correcting both misidentified peaks and over-quantification of compound concentrations found using the standard configuration alone. The 1995 data set also allows an examination of the increased complexity versus the benefits of the system modification. 6 figs., 1 tab.« less

Harnessing mass differential confinement effects in magnetized rotating plasmas to address new separation needs

NASA Astrophysics Data System (ADS)

Gueroult, R.; Rax, J.-M.; Zweben, S. J.; Fisch, N. J.

2018-01-01

The ability to separate large volumes of mixed species based on atomic mass appears desirable for a variety of emerging applications with high societal impact. One possibility to meet this objective consists in leveraging mass differential effects in rotating plasmas. Beyond conventional centrifugation, rotating plasmas offer in principle additional ways to separate elements based on mass. Single ion orbits show that ion radial mass separation in a uniform magnetized plasma column can be achieved by applying a tailored electric potential profile across the column, or by driving a rotating magnetic field within the column. Furthermore, magnetic pressure and centrifugal effects can be combined in a non-uniform geometry to separate ions based on mass along the field lines. Practical application of these separation schemes hinges on the ability to produce the desirable electric and magnetic field configuration within the plasma column.

Optimized anion exchange column isolation of zirconium-89 ( 89Zr) from yttrium cyclotron target: Method development and implementation on an automated fluidic platform

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

O’Hara, Matthew J.; Murray, Nathaniel J.; Carter, Jennifer C.

Zirconium-89 ( 89Zr), produced by the (p, n) reaction from naturally monoisotopic yttrium ( natY), is a promising positron emitting isotope for immunoPET imaging. Its long half-life of 78.4 h is sufficient for evaluating slow physiological processes. A prototype automated fluidic system, coupled to on-line and in-line detectors, has been constructed to facilitate development of new 89Zr purification methodologies. The highly reproducible reagent delivery platform and near-real time monitoring of column effluents allows for efficient method optimization. The separation of Zr from dissolved Y metal targets was evaluated using several anion exchange resins. Each resin was evaluated against its abilitymore » to quantitatively capture Zr from a load solution high in dissolved Y. The most appropriate anion exchange resin for this application was identified, and the separation method was optimized. The method is capable of a high Y decontamination factor (>10 5) and has been shown to remove Fe, an abundant contaminant in Y foils, from the 89Zr elution fraction. Finally, the method was evaluated using cyclotron bombarded Y foil targets; the method was shown to achieve >95% recovery of the 89Zr present in the foils. The anion exchange column method described here is intended to be the first 89Zr isolation stage in a dual-column purification process.« less

Optimized anion exchange column isolation of zirconium-89 ( 89Zr) from yttrium cyclotron target: Method development and implementation on an automated fluidic platform

DOE PAGES

O’Hara, Matthew J.; Murray, Nathaniel J.; Carter, Jennifer C.; ...

2018-02-24

Zirconium-89 ( 89Zr), produced by the (p, n) reaction from naturally monoisotopic yttrium ( natY), is a promising positron emitting isotope for immunoPET imaging. Its long half-life of 78.4 h is sufficient for evaluating slow physiological processes. A prototype automated fluidic system, coupled to on-line and in-line detectors, has been constructed to facilitate development of new 89Zr purification methodologies. The highly reproducible reagent delivery platform and near-real time monitoring of column effluents allows for efficient method optimization. The separation of Zr from dissolved Y metal targets was evaluated using several anion exchange resins. Each resin was evaluated against its abilitymore » to quantitatively capture Zr from a load solution high in dissolved Y. The most appropriate anion exchange resin for this application was identified, and the separation method was optimized. The method is capable of a high Y decontamination factor (>10 5) and has been shown to remove Fe, an abundant contaminant in Y foils, from the 89Zr elution fraction. Finally, the method was evaluated using cyclotron bombarded Y foil targets; the method was shown to achieve >95% recovery of the 89Zr present in the foils. The anion exchange column method described here is intended to be the first 89Zr isolation stage in a dual-column purification process.« less

Enantiomeric separation of six chiral pesticides that contain chiral sulfur/phosphorus atoms by supercritical fluid chromatography.

PubMed

Zhang, Lijun; Miao, Yelong; Lin, Chunmian

2018-03-01

Six chiral pesticides containing chiral sulfur/phosphorus atoms were separated by supercritical fluid chromatography with supercritical CO 2 as the main mobile phase component. The effect of the chiral stationary phase, different type and concentration of modifiers, column temperature, and backpressure on the separation efficiency was investigated to obtain the appropriate separation condition. Five chiral pesticides (isofenphos-methyl, isocarbophos, flufiprole, fipronil, and ethiprole) were baseline separated under experimental conditions, while isofenphos only obtained partial separation. The Chiralpak AD-3 column showed a better chiral separation ability than others for chiral pesticides containing chiral sulfur/phosphorus atoms. When different modifiers at the same concentration were used, the retention factor of pesticides except flufiprole decreased in the order of isopropanol, ethanol, methanol; meanwhile, the retention factor of flufiprole increased in the order of isopropanol, ethanol, methanol. For a given modifier, the retention factor and resolution decreased on the whole with the increase of its concentration. The enantiomer separation of five chiral pesticides was an "enthalpy-driven" process, and the separation factor decreased as the temperature increased. The backpressure of the mobile phase had little effect on the separation factor and resolution. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

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.

On-Chip Microfluidic Components for In Situ Analysis, Separation, and Detection of Amino Acids

NASA Technical Reports Server (NTRS)

Zheng, Yun; Getty, Stephanie; Dworkin, Jason; Balvin, Manuel; Kotecki, Carl

2013-01-01

The Astrobiology Analytical Laboratory at GSFC has identified amino acids in meteorites and returned cometary samples by using liquid chromatography-electrospray ionization time-of-flight mass spectrometry (LCMS). These organic species are key markers for life, having the property of chirality that can be used to distinguish biological from non-biological amino acids. One of the critical components in the benchtop instrument is liquid chromatography (LC) analytical column. The commercial LC analytical column is an over- 250-mm-long and 4.6-mm-diameter stainless steel tube filled with functionized microbeads as stationary phase to separate the molecular species based on their chemistry. Miniaturization of this technique for spaceflight is compelling for future payloads for landed missions targeting astrobiology objectives. A commercial liquid chromatography analytical column consists of an inert cylindrical tube filled with a stationary phase, i.e., microbeads, that has been functionalized with a targeted chemistry. When analyte is sent through the column by a pressurized carrier fluid (typically a methanol/ water mixture), compounds are separated in time due to differences in chemical interactions with the stationary phase. Different species of analyte molecules will interact more strongly with the column chemistry, and will therefore take longer to traverse the column. In this way, the column will separate molecular species based on their chemistry. A lab-on-chip liquid analysis tool was developed. The microfluidic analytical column is capable of chromatographically separating biologically relevant classes of molecules based on their chemistry. For this analytical column, fabrication, low leak rate, and stationary phase incorporation of a serpentine microchannel were demonstrated that mimic the dimensions of a commercial LC column within a 5 10 1 mm chip. The microchannel in the chip has a 75- micrometer-diameter oval-shaped cross section. The serpentine microchannel has four different lengths: 40, 60, 80, and 100 mm. Functionized microbeads were filled inside the microchannel to separate molecular species based on their chemistry.

Evaluation of results of cell electrophoresis experiments on space shuttle STS-3 including pre-flight and post-flight laboratory experiments

NASA Technical Reports Server (NTRS)

Todd, P. W.

1985-01-01

The objectives of the red blood cell experiments were to provide a visual check on the electrophoretic process and especially electroosmotic flow in space as well as to provide test separations of non-degradable standard particles for comparison with the separations of the three viable cell types studied on the Apollo-Soyuz Test Project. Determination of the maximum concentrations of cells that can be separated in column electrophore was a significant goal. Two of the eight columns were available for red cell experiments, so two concentrations of human and rabbit RBC mixtures were used. The objectives of another experiment were to evaluate the reproducibility of microgravity electrophoretic separation of living kidney cells, to separate cells with highly viability despite two freeze-thaw cycles, and to optimize the physical conditions of cell separation. Owing to the uncertain heterogeneity of the starting material, the experimental design does not assess resolution in microgravity, but improved separability was sought in comparison to density-gradient electrophoresis or continuous-flow electrophoresis. Efforts were made to increase cell yield and cell viability and to assess reproducibility directly.

Detection of processed genetically modified food using CIM monolithic columns for DNA isolation.

PubMed

Jerman, Sergej; Podgornik, Ales; Cankar, Katarina; Cadet, Neza; Skrt, Mihaela; Zel, Jana; Raspor, Peter

2005-02-11

The availability of sufficient quantities of DNA of adequate quality is crucial in polymerase chain reaction (PCR)-based methods for genetically modified food detection. In this work, the suitability of anion-exchange CIM (Convective Interaction Media; BIA Separations, Ljubljana, Slovenia) monolithic columns for isolation of DNA from food was studied. Maize and its derivates corn meal and thermally pretreated corn meal were chosen as model food. Two commercially available CIM disk columns were tested: DEAE (diethylaminoethyl) and QA (quaternary amine). Preliminary separations were performed with standard solution of salmon DNA at different pH values and different NaCl concentrations in mobile phase. DEAE groups and pH 8 were chosen for further isolations of DNA from a complex matrix-food extract. The quality and quantity of isolated DNA were tested on agarose gel electrophoresis, with UV-scanning spectrophotometry, and by amplification with real-time PCR. DNA isolated in this way was of suitable quality for further PCR analyses. The described method is also applicable for DNA isolation from processed foods with decreased DNA content. Furthermore, it is more effective and less time-consuming in comparison with the existing proposed methods for isolation of DNA from plant-derived foods.

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

PubMed

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

2008-07-01

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

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

PubMed Central

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

2008-01-01

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

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

Selection of stationary phase particle geometry using X-ray computed tomography and computational fluid dynamics simulations.

PubMed

Schmidt, Irma; Minceva, Mirjana; Arlt, Wolfgang

2012-02-17

The X-ray computed tomography (CT) is used to determine local parameters related to the column packing homogeneity and hydrodynamics in columns packed with spherically and irregularly shaped particles of same size. The results showed that the variation of porosity and axial dispersion coefficient along the column axis is insignificant, compared to their radial distribution. The methodology of using the data attained by CT measurements to perform a CFD simulation of a batch separation of model binary mixtures, with different concentration and separation factors is demonstrated. The results of the CFD simulation study show that columns packed with spherically shaped particles provide higher yield in comparison to columns packed with irregularly shaped particles only below a certain value of the separation factor. The presented methodology can be used for selecting a suited packing material for a particular separation task. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of strontium-90 in deer bones by liquid scintillation spectrometry after separation on Sr-specific ion exchange columns.

PubMed

Landstetter, Claudia; Wallner, Gabriele

2006-01-01

The activity concentration of (90)Sr was determined in several deer bones from Austria. Strontium specific ion exchange columns with 4',4''(5'')-di-t-butylcyclohexane-18-crown-6 from Eichrom Industries, Inc. were used for separation. The yield of the chemical procedure was quantified with AAS. Directly after column separation, the solution containing (90)Sr was mixed with the scintillation cocktail HiSafe III and measured by liquid scintillation counting. Prevention of (210)Pb contamination and reusability of the separation columns was investigated as well as the activity distribution within the bones. Results were compared with pre-Chernobyl measurements in Austria; a correlation between activity concentration of (90)Sr and site altitude was found.

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.

Short communication: separation and quantification of caseins and casein macropeptide using ion-exchange chromatography.

PubMed

Holland, B; Rahimi Yazdi, S; Ion Titapiccolo, G; Corredig, M

2010-03-01

The aim of this work was to improve an existing method to separate and quantify the 4 major caseins from milk samples (i.e., containing whey proteins) using ion-exchange chromatography. The separation process was carried out using a mini-preparative cation exchange column (1 or 5mL of column volume), using urea acetate as elution buffer at pH 3.5 with a NaCl gradient. All 4 major caseins were separated, and the purity of each peak was assessed using sodium dodecyl sulfate-PAGE. Purified casein fractions were also added to raw milk to confirm their elution volumes. The quantification was carried out using purified caseins in buffer as well as added directly to fresh skim milk. This method can also be employed to determine the decrease in kappa-casein and the release of the casein-macropeptide during enzymatic hydrolysis using rennet. In this case, the main advantage of using this method is the lack of organic solvents compared with the conventional method for separation of macropeptide (using reversed phase HPLC).

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%.

Proline-coated column for the capillary electrochromatographic separation of amino acids by in-column derivatization.

PubMed

Lin, Chun-Chi; Liu, Chuen-Ying

2004-10-01

With 3-trimethoxysilylpropyl chloride as the spacer, a proline-coated capillary column was prepared for the capillary electrochromatographic (CEC) separation of amino acids by in-column derivatization. Nine standard mixtures, including aspartic acid, glutamic acid, valine, phenylalanine, alanine, isoleucine, leucine, tyrosine, and tryptophan, were injected. o-Phthalaldehyde (OPA), OPA/2-mercaptoethanol (2-ME) and OPA/N-acetylcysteine (NAC) in borate buffer were tested as the derivatizing agent. Among them, OPA (50 mM) in borate buffer (pH 9.5, 50 mM) gave the best performance. The formation of isoindole could be detected by UV detection. The sandwich-type injection was carried out in hydrostatic mode (10 cm) with the program R(10 s)S(10 s) R(10 s)W(10 min) with R, S, and W being the reagent, sample, and waiting times. Mesityl oxide, benzyl alcohol, and acetone showed some interaction with the column. A current monitoring method was used instead of the determination of the electroosmotic flow (EOF). The direction of EOF was from anode to cathode even under acidic condition lower than the pI value (6.31) of the bonded group due to some unreacted silanol groups. Some parameters including pH, nature, and concentration of the mobile phase and the effect of organic modifier with regard to the CEC separation were investigated. With the proline-coated column (75 (50) cm x 75 microm ID) the best separation was performed in phosphate buffer (pH 4.00, 100 mM) with an applied voltage of -15 kV. The established method was also compared with those precolumn derivatized prior to the separation with proline-coated column as well as with in-capillary derivatization and separation with a bare fused-silica column. Copyright 2004 WILEY-VCH Verlag GmbH & Co.

Process and apparatus for separating fine particles by microbubble flotation together with a process and apparatus for generation of microbubbles

DOEpatents

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

1991-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine particles, especially coal, so as to produce a high purity and large recovery efficiently. This is accomplished through the use of a high aspect ratio flotation column, microbubbles, and a countercurrent use of wash water to gently wash the froth. Also, disclosed are unique processes and apparatus for generating microbubbles for flotation in a high efficient and inexpensive manner using either a porous tube or an in-line static generator. 23 figures.

Isolation of Three Components from Spearmint Oil: An Exercise in Column and Thin-Layer Chromatography

ERIC Educational Resources Information Center

Davies, Don R.; Johnson, Todd M.

2007-01-01

A simple experiment for undergraduate organic chemistry students to separate a colorless mixture using column chromatography and then monitor the outcome of the separation using thin-layer chromatography (TLC) and infrared spectroscopy(IR) is described. The experiment teaches students the principle and techniques of column and thin-layer…

Colorful Column Chromatography: A Classroom Demonstration of a Three-Component Separation

ERIC Educational Resources Information Center

Heumann, Lars V.

2008-01-01

A classroom demonstration detailing the procedure for the separation of a ternary mixture consisting of intensely colored compounds using silica gel column chromatography is described. The audience can follow the compounds during their passage through the column as individual, colored bands while learning about different tools and techniques used…

Development of a slicing device for Apollo-Soyuz Test Project (ASTP) electrophoresis technology experiment MA-011

NASA Technical Reports Server (NTRS)

Nerren, B. H.

1977-01-01

The electrophoresis of six columns was accomplished on the Apollo-Soyuz test Project. After separation, these columns were frozen in orbit and were returned for ground-based analyses. One major goal of the MA-011 experiment was the assessment of the separation achieved in orbit by slicing these frozen columns. The slicing of the frozen columns required a new device. The development of that device is described.

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

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.

Separative analyses of a chromatographic column packed with a core-shell adsorbent for lithium isotope separation

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

Sugiyama, T.; Sugura, K.; Enokida, Y.

2015-03-15

Lithium-6 is used as a blanket material for sufficient tritium production in DT fueled fusion reactors. A core-shell type adsorbent was proposed for lithium isotope separation by chromatography. The mass transfer model in a chromatographic column consisted of 4 steps, such as convection and dispersion in the column, transfer through liquid films, intra-particle diffusion and and adsorption or desorption at the local adsorption sites. A model was developed and concentration profiles and time variation in the column were numerically simulated. It became clear that core-shell type adsorbents with thin porous shell were saturated rapidly relatively to fully porous one andmore » established a sharp edge of adsorption band. This is very important feature because lithium isotope separation requires long-distance development of adsorption band. The values of HETP (Height Equivalent of a Theoretical Plate) for core-shell adsorbent packed column were estimated by statistical moments of the step response curve. The value of HETP decreased with the thickness of the porous shell. A core-shell type adsorbent is, then, useful for lithium isotope separation. (authors)« less

Microfluidic chip for peptide analysis with an integrated HPLC column, sample enrichment column, and nanoelectrospray tip.

PubMed

Yin, Hongfeng; Killeen, Kevin; Brennen, Reid; Sobek, Dan; Werlich, Mark; van de Goor, Tom

2005-01-15

Current nano-LC/MS systems require the use of an enrichment column, a separation column, a nanospray tip, and the fittings needed to connect these parts together. In this paper, we present a microfabricated approach to nano-LC, which integrates these components on a single LC chip, eliminating the need for conventional LC connections. The chip was fabricated by laminating polyimide films with laser-ablated channels, ports, and frit structures. The enrichment and separation columns were packed using conventional reversed-phase chromatography particles. A face-seal rotary valve provided a means for switching between sample loading and separation configurations with minimum dead and delay volumes while allowing high-pressure operation. The LC chip and valve assembly were mounted within a custom electrospray source on an ion-trap mass spectrometer. The overall system performance was demonstrated through reversed-phase gradient separations of tryptic protein digests at flow rates between 100 and 400 nL/min. Microfluidic integration of the nano-LC components enabled separations with subfemtomole detection sensitivity, minimal carryover, and robust and stable electrospray throughout the LC solvent gradient.

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

Light water detritiation

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

Fedorchenko, O.A.; Aleksee, I.A.; Bondarenko, S.D.

2015-03-15

Hundreds of thousands of tons of tritiated light water have been accumulating from the enterprises of nuclear fuel cycles around the world. The Dual-Temperature Water-Hydrogen (DTWH) process looks like the only practical alternative to Combined Electrolysis and Catalytic Exchange (CECE). In DTWH power-consuming lower reflux device (electrolytic cell) is replaced by a so-called 'hot tower' (LPCE column operating at conditions which ensure relatively small value of elementary separation factor α(hot)). In the upper, cold tower, the tritium transfers from hydrogen to water while in the lower, hot tower - in the opposite direction - from water to hydrogen. The DTWHmore » process is much more complicated compared to CECE; it must be thoroughly computed and strictly controlled by an automatic control system. The use of a simulation code for DTWH is absolutely important. The simulation code EVIO-5 deals with 3 flows inside a column (hydrogen gas, water vapour and liquid water) and 2 simultaneous isotope exchange sub-processes (counter-current phase exchange and co-current catalytic exchange). EVIO-5 takes into account the strong dependence of process performance on given conditions (temperature and pressure). It calculates steady-state isotope concentration profiles considering a full set of reversible exchange reactions between different isotope modifications of water and hydrogen (12 molecular species). So the code can be used for simulation of LPCE column operation for detritiation of hydrogen and water feed, which contains H and D not only at low concentrations but above 10 at.% also. EVIO-5 code is used to model a Tritium Removal Facility with a throughput capacity of about 400 m{sup 3}/day. Simulation results show that a huge amount of wet-proofed catalyst is required (about 6000 m{sup 3}), mainly (90%) in the first stage. One reason for these large expenses (apart from a big scale of the problem itself) is the relatively high tritium separation factor in the hot tower. The introduction of some quantity of deuterium into the gaseous flow before the hot tower lowers the tritium separation factor in that column. One possible variant of deuterium introduction to the hot tower of the first stage was modelled. The decontamination capacity increases by a 2.5 factor.« less

Automated gas chromatography

DOEpatents

Mowry, C.D.; Blair, D.S.; Rodacy, P.J.; Reber, S.D.

1999-07-13

An apparatus and process for the continuous, near real-time monitoring of low-level concentrations of organic compounds in a liquid, and, more particularly, a water stream. A small liquid volume of flow from a liquid process stream containing organic compounds is diverted by an automated process to a heated vaporization capillary where the liquid volume is vaporized to a gas that flows to an automated gas chromatograph separation column to chromatographically separate the organic compounds. Organic compounds are detected and the information transmitted to a control system for use in process control. Concentrations of organic compounds less than one part per million are detected in less than one minute. 7 figs.

Automated gas chromatography

DOEpatents

Mowry, Curtis D.; Blair, Dianna S.; Rodacy, Philip J.; Reber, Stephen D.

1999-01-01

An apparatus and process for the continuous, near real-time monitoring of low-level concentrations of organic compounds in a liquid, and, more particularly, a water stream. A small liquid volume of flow from a liquid process stream containing organic compounds is diverted by an automated process to a heated vaporization capillary where the liquid volume is vaporized to a gas that flows to an automated gas chromatograph separation column to chromatographically separate the organic compounds. Organic compounds are detected and the information transmitted to a control system for use in process control. Concentrations of organic compounds less than one part per million are detected in less than one minute.

Prototype of an Interface for Hyphenating Distillation with Gas Chromatography and Mass Spectrometry

PubMed Central

Tang, Ya-Ru; Yang, Hui-Hsien; Urban, Pawel L.

2017-01-01

Chemical analysis of complex matrices—containing hundreds of compounds—is challenging. Two-dimensional separation techniques provide an efficient way to reduce complexity of mixtures analyzed by mass spectrometry (MS). For example, gasoline is a mixture of numerous compounds, which can be fractionated by distillation techniques. However, coupling conventional distillation with other separations as well as MS is not straightforward. We have established an automatic system for online coupling of simple microscale distillation with gas chromatography (GC) and electron ionization MS. The developed system incorporates an interface between the distillation condenser and the injector of a fused silica capillary GC column. Development of this multidimensional separation (distillation-GC-MS) was preceded by a series of preliminary off-line experiments. In the developed technique, the components with different boiling points are fractionated and instantly analyzed by GC-MS. The obtained data sets illustrate dynamics of the distillation process. An important advantage of the distillation-GC-MS technique is that raw samples can directly be analyzed without removal of the non-volatile matrix residues that could contaminate the GC injection port and the column. Distilling the samples immediately before the injection to the GC column may reduce possible matrix effects—especially in the early phase of separation, when molecules with different volatilities co-migrate. It can also reduce losses of highly volatile components (during fraction collection and transfer). The two separation steps are partly orthogonal, what can slightly increase selectivity of the entire analysis. PMID:28337400

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.

Use of a polar ionic liquid as second column for the comprehensive two-dimensional GC separation of PCBs.

PubMed

Zapadlo, Michal; Krupcík, Ján; Májek, Pavel; Armstrong, Daniel W; Sandra, Pat

2010-09-10

The orthogonality of three columns coupled in two series was studied for the congener specific comprehensive two-dimensional GC separation of polychlorinated biphenyls (PCBs). A non-polar capillary column coated with poly(5%-phenyl-95%-methyl)siloxane was used as the first ((1)D) column in both series. A polar capillary column coated with 70% cyanopropyl-polysilphenylene-siloxane or a capillary column coated with the ionic liquid 1,12-di(tripropylphosphonium)dodecane bis(trifluoromethane-sulfonyl)imide were used as the second ((2)D) columns. Nine multi-congener standard PCB solutions containing subsets of all native 209 PCBs, a mixture of 209 PCBs as well as Aroclor 1242 and 1260 formulations were used to study the orthogonality of both column series. Retention times of the corresponding PCB congeners on (1)D and (2)D columns were used to construct retention time dependences (apex plots) for assessing orthogonality of both columns coupled in series. For a visual assessment of the peak density of PCBs congeners on a retention plane, 2D images were compared. The degree of orthogonality of both column series was, along the visual assessment of distribution of PCBs on the retention plane, evaluated also by Pearson's correlation coefficient, which was found by correlation of retention times t(R,i,2D) and t(R,i,1D) of corresponding PCB congeners on both column series. It was demonstrated that the apolar+ionic liquid column series is almost orthogonal both for the 2D separation of PCBs present in Aroclor 1242 and 1260 formulations as well as for the separation of all of 209 PCBs. All toxic, dioxin-like PCBs, with the exception of PCB 118 that overlaps with PCB 106, were resolved by the apolar/ionic liquid series while on the apolar/polar column series three toxic PCBs overlapped (105+127, 81+148 and 118+106). Copyright 2010 Elsevier B.V. All rights reserved.

ENANTIOMER SEPARATION OF POLYCHLORINATED BIPHENYL ATROPISOMERS AND POLYCHLORINATED BIPHENYL RETENTION BEHAVIOR ON MODIFIED CYCLODEXTRIN CAPILLARY GAS CHROMATOGRAPHY COLUMNS

EPA Science Inventory

Seven commercially-available chiral capillary gas chromatography columns containing modified cyclodextrins were evaluated for their ability to separate enantiomers of the 19 stable chiral polychlorinated biphenyl (PCB) atropisomers, and for their ability to separate these enantio...

SEPARATION OF OCTYLPHENOL POLYETHER ALCOHOLS SURFACTANTS BY CAPILLARY COLUMN AND HPLC

EPA Science Inventory

Separation of nonionic octylphenol polyether alcohols (OPA) by supercritical fluid chromatography (SFC) and HPLC is described. sing a density programming and a 50-pm i.d. capillary column, a total of 18 group oligomers was separated. he effects of the operating parameters, such a...

Evaluation of comprehensive multidimensional separations using reversed-phase, reversed-phase liquid chromatography/mass spectrometry for shotgun proteomics.

PubMed

Nakamura, Tatsuji; Kuromitsu, Junro; Oda, Yoshiya

2008-03-01

Two-dimensional liquid-chromatographic (LC) separation followed by mass spectrometric (MS) analysis was examined for the identification of peptides in complex mixtures as an alternative to widely used two-dimensional gel electrophoresis followed by MS analysis for use in proteomics. The present method involves the off-line coupling of a narrow-bore, polymer-based, reversed-phase column using an acetonitrile gradient in an alkaline mobile phase in the first dimension with octadecylsilanized silica (ODS)-based nano-LC/MS in the second dimension. After the first separation, successive fractions were acidified and dried off-line, then loaded on the second dimension column. Both columns separate peptides according to hydrophobicity under different pH conditions, but more peptides were identified than with the conventional technique for shotgun proteomics, that is, the combination of a strong cation exchange column with an ODS column, and the system was robust because no salts were included in the mobile phases. The suitability of the method for proteomics measurements was evaluated.

Comprehensive two-dimensional chromatography with coupling of reversed phase high performance liquid chromatography and supercritical fluid chromatography.

PubMed

Stevenson, Paul G; Tarafder, Abhijit; Guiochon, Georges

2012-01-13

A 2D comprehensive chromatographic separation of blackberry sage fragrant oil was performed by using HPLC in the first dimension and SFC in the second. A C(18)-bonded silica column eluted with an ACN gradient was used in the HPLC dimension and an amino-bonded silica column eluted with ACN as a modifier in the SFC dimension. This 2D separation was completed in the off-line mode, the fractions from the HPLC column being collected and injected in the SFC column. The retention factors on the two columns have a -0.757 correlation coefficient. The method provides a practical peak capacity of 2400 in 280 min. The first eluted peaks in HPLC are the last ones eluted in SFC and vice versa. The results demonstrate that the coupling of an HPLC and an SFC separation have a great potential for 2D chromatographic separations. Copyright © 2011 Elsevier B.V. All rights reserved.

Filtrates and Residues: Chlorophyll Separation and Spectral Identification.

ERIC Educational Resources Information Center

Diehl-Jones, Susan M.

1984-01-01

Describes an experiment in which students become familiar with the organic chemistry extraction process, perform analyses by thin layer and column chromatography, and use the absorption spectrum (obtained from a spectrophotometer) for identification. List of materials needed and procedures used are provided. (JN)

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

Establishing column batch repeatability according to Quality by Design (QbD) principles using modeling software.

PubMed

Rácz, Norbert; Kormány, Róbert; Fekete, Jenő; Molnár, Imre

2015-04-10

Column technology needs further improvement even today. To get information of batch-to-batch repeatability, intelligent modeling software was applied. Twelve columns from the same production process, but from different batches were compared in this work. In this paper, the retention parameters of these columns with real life sample solutes were studied. The following parameters were selected for measurements: gradient time, temperature and pH. Based on calculated results, batch-to-batch repeatability of BEH columns was evaluated. Two parallel measurements on two columns from the same batch were performed to obtain information about the quality of packing. Calculating the average of individual working points at the highest critical resolution (R(s,crit)) it was found that the robustness, calculated with a newly released robustness module, had a success rate >98% among the predicted 3(6) = 729 experiments for all 12 columns. With the help of retention modeling all substances could be separated independently from the batch and/or packing, using the same conditions, having high robustness of the experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

Optimized anion exchange column isolation of zirconium-89 (89Zr) from yttrium cyclotron target: Method development and implementation on an automated fluidic platform.

PubMed

O'Hara, Matthew J; Murray, Nathaniel J; Carter, Jennifer C; Morrison, Samuel S

2018-04-13

Zirconium-89 ( 89 Zr), produced by the (p, n) reaction from naturally monoisotopic yttrium ( nat Y), is a promising positron emitting isotope for immunoPET imaging. Its long half-life of 78.4 h is sufficient for evaluating slow physiological processes. A prototype automated fluidic system, coupled to on-line and in-line detectors, has been constructed to facilitate development of new 89 Zr purification methodologies. The highly reproducible reagent delivery platform and near-real time monitoring of column effluents allows for efficient method optimization. The separation of Zr from dissolved Y metal targets was evaluated using several anion exchange resins. Each resin was evaluated against its ability to quantitatively capture Zr from a load solution high in dissolved Y. The most appropriate anion exchange resin for this application was identified, and the separation method was optimized. The method is capable of a high Y decontamination factor (>10 5 ) and has been shown to remove Fe, an abundant contaminant in Y foils, from the 89 Zr elution fraction. Finally, the method was evaluated using cyclotron bombarded Y foil targets; the method was shown to achieve >95% recovery of the 89 Zr present in the foils. The anion exchange column method described here is intended to be the first 89 Zr isolation stage in a dual-column purification process. Copyright © 2018 Elsevier B.V. All rights reserved.

Ionic liquid phases with comprehensive two-dimensional gas chromatography of fatty acid methyl esters.

PubMed

Pojjanapornpun, Siriluck; Nolvachai, Yada; Aryusuk, Kornkanok; Kulsing, Chadin; Krisnangkura, Kanit; Marriott, Philip J

2018-02-17

New generation inert ionic liquid (iIL) GC columns IL60i, IL76i and IL111i, comprising phosphonium or imidazolium cationic species, were investigated for separation of fatty acid methyl esters (FAME). In general, the iIL phases provide comparable retention times to their corresponding conventional columns, with only minor selectivity differences. The average tailing factors and peak widths were noticeably improved (reduced) for IL60i and IL76i, while they were slightly improved for IL111i. Inert IL phase columns were coupled with conventional IL columns in comprehensive two-dimensional GC (GC × GC) with a solid-state modulator which offers variable modulation temperature (T M ), programmable T M during analysis and trapping stationary phase material during the trap/release (modulation) process, independent of oven T and column sets. Although IL phases are classified as polar, relative polarity of the two phases comprising individual GC × GC column sets permits combination of less-polar IL/polar IL and polar IL/less-polar IL column sets; it was observed that a polar/less-polar column set provided better separation of FAME. A higher first dimension ( 1 D) phase polarity combined with a lower 2 D phase polarity, for instance 1 D IL111i with 2 D IL59 gave the best result; the greater difference in 1 D/ 2 D phase polarity results in increasing occupancy of peak area in the 2D space. The IL111i/IL59 column set was selected for analysis of fatty acids in fat and oil products (butter, margarine, fish oil and canola oil). Compared with the conventional IL111, IL111i showed reduced column bleed which makes this more suited to GC × GC analysis of FAME. The proposed method offers a fast profiling approach with good repeatability of analysis of FAME.

Separation of Albumin, Ceruloplasmin, and Transferrin from Human Plasma.

ERIC Educational Resources Information Center

Barnes, Grady; Frieden, Earl

1982-01-01

Procedures are provided for separating the principal metalloproteins (albumin, ceruloplasmin, and transferrin) from plasma using column chromatographic techniques. The experiment can be completed in two separate three-hour laboratory periods during which column chromatography is illustrated and the effect of pH on charge and affinity of a protein…

Radial Chromatography for the Separation of Nitroaniline Isomers

ERIC Educational Resources Information Center

Miller, Robert B.; Case, William S.

2011-01-01

Separation techniques are usually presented in the undergraduate organic laboratory to teach students how to purify and isolate compounds. Often the concept of liquid chromatography is introduced by having students create "silica gel columns" to separate components of a reaction mixture. Although useful, column chromatography can be a laborious…

EFFECTS OF TEMPERATURE AND SOLVENT COMPOSITION ON THE CHIRALCEL OJ SEPARATION OF CHIRAL ORGANOPHOSPHORUS PESTICIDES

EPA Science Inventory

The separation of the enantiomers of twelve organophosphorus pesticides (OPs) was investigated on the CHIRALCEL?OJ column to determine whether the mobile phase composition, flow rate and column temperature could be optimized to yield at least partial separation of the enantiomers...

SEPARATION OF OCTYLPHENOL POLYETHER ALCOHOLS SURFACTANTS BY CAPILLARY COLUMN SFC AND HPLC

EPA Science Inventory

Separation of nonionic octylphenol polyether alcohols (OPA) by supercritical fluid chromatography (SFC) and HPLC is described. Using a density programming and a 50-μm i.d. capillary column, a total of 18 group oligomers was separated. The effects of the operating parameters, such...

Aspects regarding at 13C isotope separation column control using Petri nets system

NASA Astrophysics Data System (ADS)

Boca, M. L.; Ciortea, M. E.

2015-11-01

This paper is intended to show that Petri nets can be also applicable in the chemical industry. It used linear programming, modeling underlying Petri nets, especially discrete event systems for isotopic separation, the purpose of considering and control events in real-time through graphical representations. In this paper it is simulate the control of 13C Isotope Separation column using Petri nets. The major problem with 13C comes from the difficulty of obtaining it and raising its natural fraction. Carbon isotopes can be obtained using many methods, one of them being the cryogenic distillation of carbon monoxide. Some few aspects regarding operating conditions and the construction of such cryogenic plants are known today, and even less information are available as far as the separation process modeling and control are concerned. In fact, the efficient control of the carbon monoxide distillation process represents a necessity for large-scale 13C production. Referring to a classic distillation process, some models for carbon isotope separation have been proposed, some based on mass, component and energy balance equations, some on the nonlinear wave theory or the Cohen equations. For modeling the system it was used Petri nets because in this case it is deal with discrete event systems. In use of the non-timed and with auxiliary times Petri model, the transport stream was divided into sections and these sections will be analyzed successively. Because of the complexity of the system and the large amount of calculations required it was not possible to analyze the system as a unitary whole. A first attempt to model the system as a unitary whole led to the blocking of the model during simulation, because of the large processing times.

Preparative liquid column electrophoresis of T and B lymphocytes at gravity = 1

NASA Technical Reports Server (NTRS)

Van Oss, C. J.; Bigazzi, P. E.; Gillman, C. F.; Allen, R. E.

1974-01-01

Vertical liquid columns containing low-molecular-weight dextran density gradients can be used for preparative lymphocyte electrophoresis on earth, in simulation of zero gravity conditions. Another method that has been tested at 1 g, is the electrophoresis of lymphocytes in an upward direction in vertical columns. By both methods up to 100 million lymphocytes can be separated at one time in a 30-cm glass column of 8-mm inside diameter, at 12 V/cm, in two hours. Due to convection and sedimentation problems, the separation at 1 g is less than ideal, but it is expected that at zero gravity electrophoresis will probe to be a uniquely powerful cell separation tool.

Integrated Extraction Chromatographic Separation of the Lithophile Elements Involved in Long-Lived Radiogenic Isotope Systems (Rb-Sr, U-Th-Pb, Sm-Nd, La-Ce, and Lu-Hf) Useful in Geochemical and Environmental Sciences.

PubMed

Pin, Christian; Gannoun, Abdelmouhcine

2017-02-21

A fast and efficient sample preparation method in view of isotope ratio measurements is described, allowing the separation of 11 elements involved, either as "parent" or as "daughter" isotopes, in six radiogenic isotope systems used as chronometers and tracers in earth, planetary, and environmental sciences. The protocol is based on small extraction chromatographic columns, used either alone or in tandem, through which a single nitric acid solution is passed, without any intervening evaporation step. The columns use commercially available extraction resins (Sr resin, TRU resin, Ln resin, RE resin, and again Ln resin for isolating Sr and Pb, LREE then La-Ce-Nd-Sm, Lu(Yb), and Hf, Th, and U, respectively) along with an additional, in-house prepared resin for separating Rb. A simplified scheme is proposed for samples requiring the separation of Sr, Pb, Nd, and Hf only. Adverse effects of troublesome major elements (Fe 3+ , Ti) are circumvented by masking with ascorbic acid and hydrofluoric acid, respectively. Typical recoveries in the 85-95% range are achieved, with procedural blanks of 10-100 pg, negligible with regard to the amounts of analytes processed. The fractions separated are suitable for high precision isotope ratio measurements by TIMS or MC-ICP-MS, as demonstrated by the repeat analyses of several international reference materials of basaltic composition for 87 Sr/ 86 Sr, 208,207,206 Pb/ 204 Pb, 143 Nd/ 144 Nd, 176 Hf/ 177 Hf, and 230 Th/ 232 Th. Concentration data could be obtained by spiking and equilibrating the sample with appropriate isotopic tracers before the onset of the separation process and, finally, measuring the isotope ratios modified by the isotope dilution process.

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

PubMed

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

2013-01-01

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

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.

Isotopic generator for bismuth-212 and lead-212 based on radium

DOEpatents

Hines, J.J.; Atcher, R.W.; Friedman, A.M.

1985-01-30

Disclosed are method and apparatus for providing radionuclides of bismuth-212 and lead-212. Thorium-228 and carrier solution starting material is input to a radiologically contained portion of an isotopic generator system, and radium-224 is separated from thorium-228 which is retained by a strongly basic anion exchange column. The separated radium-224 is transferred to an accessible, strongly acidic cationic exchange column. The cationic column retains the radium-224, and natural radioactive decay generates bismuth-212 and lead-212. The cationic exchange column can also be separated from the contained portion of the system and utilized without the extraordinary safety measures necessary in the contained portion. Furthermore, the cationic exchange column provides over a relatively long time period the short lived lead-212 and bismuth-212 radionuclides which are useful for a variety of medical therapies.

Isotopic generator for bismuth-212 and lead-212 from radium

DOEpatents

Atcher, Robert W.; Friedman, Arnold M.; Hines, John

1987-01-01

A method and apparatus for providing radionuclides of bismuth-212 and lead-212. Thorium-228 and carrier solution starting material is input to a radiologically contained portion of an isotopic generator system, and radium-224 is separated from thorium-228 which is retained by a strongly basic anion exchange column. The separated radium-224 is transferred to an accessible, strongly acidic cationic exchange column. The cationic column retains the radium-224, and natural radioactive decay generates bismuth-212 and lead-212. The cationic exchange column can also be separated from the contained portion of the system and utilized without the extraordinary safety measures necessary in the contained portion. Furthermore, the cationic exchange column provides over a relatively long time period the short lived lead-212 and bismuth-212 radionuclides which are useful for a variety of medical therapies.

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.

Magnetic nanoparticles and high-speed countercurrent chromatography coupled in-line and using the same solvent system for separation of quercetin-3-O-rutinoside, luteoloside and astragalin from a Mikania micrantha extract.

PubMed

Wang, Juanqiang; Geng, Shan; Wang, Binghai; Shao, Qian; Fang, Yingtong; Wei, Yun

2017-07-28

A new in-line method of magnetic nanoparticles (MNPs) coupled with high-speed countercurrent chromatography (HSCCC) using a same solvent system during the whole separation process was established to achieve the rapid separation of flavonoids from Mikania micrantha. The adsorption and desorption capacities of five different MNPs for flavonoid standards and Mikania micrantha crude extract were compared and the most suitable magnetic nanoparticle Fe 3 O 4 @SiO 2 @DIH@EMIMLpro was selected as the in-line MNP column. An in-line separation system was established by combining this MNP column with HSCCC through a six-way valve. The comparison between two solvent systems n-hexane-ethyl acetate-methanol-water (3:5:3:5, v/v) and ethyl acetate-methanol-water (25:1:25, v/v) showed that the latter solvent system was more suitable for simultaneously in-line separating three flavonoids quercetin-3-O-rutinoside, luteoloside and astragalin from Mikania micrantha. The purities of these three compounds with the ethyl acetate-methanol-water solvent system were 95.13%, 98.54% and 98.19% respectively. Results showed the established in-line separation system of MNP-HSCCC was efficient, recyclable and served to isolate potential flavonoids with similar polarities from natural complex mixtures. The in-line combination of magnetic nanoparticles with high-speed countercurrent chromatography eluting with the same solvent system during the whole separation process was established for the first time. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

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.

Adsorption and separation of proteins by collagen fiber adsorbent.

PubMed

Li, Juan; Liao, Xue-pin; Zhang, Qi-xian; Shi, Bi

2013-06-01

The separation of proteins is a key step in biomedical and pharmaceutical industries. In the present investigation, the collagen fiber adsorbent (CFA) was exploited as column packing material to separate proteins. Bovine serum albumin (BSA), bovine hemoglobin (Hb) and lysozyme (LYS) that have different isoelectric points (pIs) were selected as model proteins to investigate the separation ability of CFA to proteins. In batch adsorption, the adsorption behaviors of these proteins on CFA under different pHs and ionic strengths indicated that the electrostatic interaction plays a predominant role in the adsorption of proteins on CFA. CFA exhibited high adsorption capacity to Hb and LYS. In column separation, the proteins were completely separated by adjusting pH and ionic strength of the eluent. The increase of flow rate could reduce the separation time with no influence on the recovery of protein in the experimental range. The protein recovery was higher than 90% even when the CFA column was re-used for 4 times in separation of BSA and LYS, and the retention time of BSA or LYS was almost constant during the repeated applications. In addition, as a practical application, LYS was successfully separated from chicken egg white powder by CFA column. Copyright © 2013 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.

Chiral stationary phase optimized selectivity liquid chromatography: A strategy for the separation of chiral isomers.

PubMed

Hegade, Ravindra Suryakant; De Beer, Maarten; Lynen, Frederic

2017-09-15

Chiral Stationary-Phase Optimized Selectivity Liquid Chromatography (SOSLC) is proposed as a tool to optimally separate mixtures of enantiomers on a set of commercially available coupled chiral columns. This approach allows for the prediction of the separation profiles on any possible combination of the chiral stationary phases based on a limited number of preliminary analyses, followed by automated selection of the optimal column combination. Both the isocratic and gradient SOSLC approach were implemented for prediction of the retention times for a mixture of 4 chiral pairs on all possible combinations of the 5 commercial chiral columns. Predictions in isocratic and gradient mode were performed with a commercially available and with an in-house developed Microsoft visual basic algorithm, respectively. Optimal predictions in the isocratic mode required the coupling of 4 columns whereby relative deviations between the predicted and experimental retention times ranged between 2 and 7%. Gradient predictions led to the coupling of 3 chiral columns allowing baseline separation of all solutes, whereby differences between predictions and experiments ranged between 0 and 12%. The methodology is a novel tool allowing optimizing the separation of mixtures of optical isomers. Copyright © 2017 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

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

PubMed

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

2010-06-04

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

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.

Comparison of GC stationary phases for the separation of fatty acid methyl esters in biodiesel fuels.

PubMed

Goding, Julian C; Ragon, Dorisanne Y; O'Connor, Jack B; Boehm, Sarah J; Hupp, Amber M

2013-07-01

The fatty acid methyl ester (FAME) content of biodiesel fuels has traditionally been determined using gas chromatography with a polar stationary phase. In this study, a direct comparison of the separation of FAMEs present in various biodiesel samples on three polar stationary phases and one moderately polar stationary phase (with comparable column dimensions) was performed. Retention on each column was based on solubility in and polarity of the phase. Quantitative metrics describing the resolution of important FAME pairs indicate high resolution on all polar columns, yet the best resolution, particularly of geometric isomers, is achieved on the cyanopropyl column. In addition, the separation of four C18 monounsaturated isomers was optimized and the elution order determined on each column. FAME composition of various biodiesel fuel types was determined on each column to illustrate (1) chemical differences in biodiesels produced from different feedstocks and (2) chemical similarities in biodiesels of the same feedstock type produced in different locations and harvest seasons.

Microgravity electrophoresis: A study of the factors that affect free-fluid separation

NASA Technical Reports Server (NTRS)

1985-01-01

Electrophoresis experiments have been performed in the microgravity environment of the Space Shuttle. Test particles (fixed human and rabbit erythrocytes) migrated as expected in a static column and test macromolecules (human serum albumin, ovalbumin, hemoglobin A, and Pneumococcus polysaccharide 6B) migrated as expected in a continuous flow apparatus. The concentrations studied exceeded those that can be used in free-fluid separation and purification processes at unit gravity.

Integrated multiplexed capillary electrophoresis system

DOEpatents

Yeung, Edward S.; Tan, Hongdong

2002-05-14

The present invention provides an integrated multiplexed capillary electrophoresis system for the analysis of sample analytes. The system integrates and automates multiple components, such as chromatographic columns and separation capillaries, and further provides a detector for the detection of analytes eluting from the separation capillaries. The system employs multiplexed freeze/thaw valves to manage fluid flow and sample movement. The system is computer controlled and is capable of processing samples through reaction, purification, denaturation, pre-concentration, injection, separation and detection in parallel fashion. Methods employing the system of the invention are also provided.

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.

Hybridation of different chiral separation techniques with ICP-MS detection for the separation and determination of selenomethionine enantiomers: chiral speciation of selenized yeast.

PubMed

Méndez, S P; González, E B; Sanz-Medel, A

2001-05-01

Enantioseparation and determination of selenomethionine enantiomers in selenized yeast was investigated using chiral separation techniques based on different principles, coupled on-line to inductively coupled plasma mass spectrometry (ICP-MS) for selenium-specific detection. High performance liquid chromatography (HPLC) on a beta-cyclodestrin (beta-CD) column, cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC), gas chromatography (GC) on a Chirasil-L-Val column, and HPLC on a Chirobiotic T column have been investigated as the chiral separation techniques. For HPLC separation on the beta-CD column, and also for CD-MEKC, selenomethionine enantiomers were derivatized with NDA/CN(-). For chiral separation by GC, selenomethionine enantiomers were converted into their N-trifluoroacetyl (TFA)-O-alkyl esters. The developed hybridation methodologies are compared with respect to enantioselectivity, sensitivity and analysis time. The usefulness of the best-suited method [HPLC (Chirobiotic T)-ICP-MS] was demonstrated by its application to the successful chiral speciation of selenium and D-and L-selenomethionine content determination in selenized yeast. Copyright 2001 John Wiley & Sons, Ltd.

Transport of Cryptosporidium parvum Oocysts in Soil Columns following Applications of Raw and Separated Liquid Slurries

PubMed Central

Petersen, Heidi H.; Enemark, Heidi L.; Olsen, Annette; Amin, M. G. Mostofa

2012-01-01

The potential for the transport of viable Cryptosporidium parvum oocysts through soil to land drains and groundwater was studied using simulated rainfall and intact soil columns which were applied raw slurry or separated liquid slurry. Following irrigation and weekly samplings over a 4-week period, C. parvum oocysts were detected from all soil columns regardless of slurry type and application method, although recovery rates were low (<1%). Soil columns with injected liquid slurry leached 73 and 90% more oocysts compared to columns with injected and surface-applied raw slurries, respectively. Among leachate samples containing oocysts, 44/72 samples yielded viable oocysts as determined by a dye permeability assay (DAPI [4′,6′-diamidino-2-phenylindole]/propidium iodide) with the majority (41%) of viable oocysts found in leachate from soil columns with added liquid slurry. The number of viable oocysts was positively correlated (r = 0.63) with the total number of oocysts found. Destructively sampling of the soil columns showed that type of slurry and irrigation played a role in the vertical distribution of oocysts, with more oocysts recovered from soil columns added liquid slurry irrespective of the irrigation status. Further studies are needed to determine the effectiveness of different slurry separation technologies to remove oocysts and other pathogens, as well as whether the application of separated liquid slurry to agricultural land may represent higher risks for groundwater contamination compared to application of raw slurry. PMID:22706058

Preparation, characterization, and performance evaluation of UiO-66 analogues as stationary phase in HPLC for the separation of substituted benzenes and polycyclic aromatic hydrocarbons

PubMed Central

Yan, Zengguang; Li, Jianrong; Xie, Yabo; Bai, Liping; Jiang, Lin; Li, Fasheng

2017-01-01

UiO-66 analogues are good candidates as stationary phase in HPLC because of their chemical/thermal stability, large surface area, and two cage structures. Here, two UiO-66 analogues, UiO-66-NH2 and UiO-67, were synthesized and used as stationary phase in HPLC to evaluate their performance in the separation of substituted benzenes (SBs) and polycyclic aromatic hydrocarbons (PAHs). The results showed that SBs could be well separated on UiO-66-NH2 column but not on UiO-67 column. Nonetheless, PAHs could be well separated on UiO-67 column. The separation mechanisms of SBs and PAHs on UiO-66 analogues may be involved in the pore size and functional group in the frameworks of UiO-66 analogues. Introduction of the–NH2 into UiO-66 significantly reduced its adsorption capacity for SB congeners, which resulted in less separation of SBs on UiO-66-NH2. As for the separation of PAHs on UiO-67 column, the π-π stacking effect was supposed to play a vital role. PMID:28582453

Preparation, characterization, and performance evaluation of UiO-66 analogues as stationary phase in HPLC for the separation of substituted benzenes and polycyclic aromatic hydrocarbons.

PubMed

Zhao, Weiwei; Zhang, Chaoyan; Yan, Zengguang; Zhou, Youya; Li, Jianrong; Xie, Yabo; Bai, Liping; Jiang, Lin; Li, Fasheng

2017-01-01

UiO-66 analogues are good candidates as stationary phase in HPLC because of their chemical/thermal stability, large surface area, and two cage structures. Here, two UiO-66 analogues, UiO-66-NH2 and UiO-67, were synthesized and used as stationary phase in HPLC to evaluate their performance in the separation of substituted benzenes (SBs) and polycyclic aromatic hydrocarbons (PAHs). The results showed that SBs could be well separated on UiO-66-NH2 column but not on UiO-67 column. Nonetheless, PAHs could be well separated on UiO-67 column. The separation mechanisms of SBs and PAHs on UiO-66 analogues may be involved in the pore size and functional group in the frameworks of UiO-66 analogues. Introduction of the-NH2 into UiO-66 significantly reduced its adsorption capacity for SB congeners, which resulted in less separation of SBs on UiO-66-NH2. As for the separation of PAHs on UiO-67 column, the π-π stacking effect was supposed to play a vital role.

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

Kojima, S.; Yokosawa, M.; Matsuyama, M.

To study the practical application of a tritium separation process using Self-Developing Gas Chromatography (SDGC) using a Pd-Pt alloy, intermediate scale-up experiments (22 mm ID x 2 m length column) and the development of a computational simulation method have been conducted. In addition, intermediate scale production of Pd-Pt powder has been developed for the scale-up experiments.The following results were obtained: (1) a 50-fold scale-up from 3 mm to 22 mm causes no significant impact on the SDGC process; (2) the Pd-Pt alloy powder is applicable to a large size SDGC process; and (3) the simulation enables preparation of a conceptualmore » design of a SDGC process for tritium separation.« less

Glycolipid class profiling by packed-column subcritical fluid chromatography.

PubMed

Deschamps, Frantz S; Lesellier, Eric; Bleton, Jean; Baillet, Arlette; Tchapla, Alain; Chaminade, Pierre

2004-06-18

The potential of packed-column subcritical fluid chromatography (SubFC) for the separation of lipid classes has been assessed in this study. Three polar stationary phases were checked: silica, diol, and poly(vinyl alcohol). Carbon dioxide (CO2) with methanol as modifier was used as mobile phase and detection performed by evaporative light scattering detection. The influence of methanol content, temperature, and pressure on the chromatographic behavior of sphingolipids and glycolipids were investigated. A complete separation of lipid classes from a crude wheat lipid extract was achieved using a modifier gradient from 10 to 40% methanol in carbon dioxide. Solute selectivity was improved using coupled silica and diol columns in series. Because the variation of eluotropic strength depending on the fluid density changes, a normalized separation factor product (NSP) was used to select the nature, the number and the order of the columns to reach the optimum glycolipid separation.

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

PubMed

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

2017-04-01

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

"Supermarket Column Chromatography of Leaf Pigments" Revisited: Simple and Ecofriendly Separation of Plant Carotenoids, Chlorophylls, and Flavonoids from Green and Red Leaves

ERIC Educational Resources Information Center

Dias, Alice M.; Ferreira, Maria La Salete

2015-01-01

A simple and ecofriendly procedure was developed in order to prepare extracts from red and green leaves. This procedure enables the separation of yellow, green, and red band pigments and optimizes the previously reported baking soda "supermarket column". The same extract also led to a novel and colorful potato starch column, which can…

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.

Investigation to biodiesel production by the two-step homogeneous base-catalyzed transesterification.

PubMed

Ye, Jianchu; Tu, Song; Sha, Yong

2010-10-01

For the two-step transesterification biodiesel production made from the sunflower oil, based on the kinetics model of the homogeneous base-catalyzed transesterification and the liquid-liquid phase equilibrium of the transesterification product, the total methanol/oil mole ratio, the total reaction time, and the split ratios of methanol and reaction time between the two reactors in the stage of the two-step reaction are determined quantitatively. In consideration of the transesterification intermediate product, both the traditional distillation separation process and the improved separation process of the two-step reaction product are investigated in detail by means of the rigorous process simulation. In comparison with the traditional distillation process, the improved separation process of the two-step reaction product has distinct advantage in the energy duty and equipment requirement due to replacement of the costly methanol-biodiesel distillation column. Copyright 2010 Elsevier Ltd. All rights reserved.

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.

Preparative separation and purification of rosmarinic acid from perilla seed meal via combined column chromatography.

PubMed

Tang, Weizhuo; Sun, Baoshan; Zhao, Yuqing

2014-02-01

In this study, the preparative separation and purification of rosmarinic acid (RA) from perilla seed meal (PSM), which is a by-product of edible oil production, was achieved using combined column chromatography over macroporous and polyamide resins. To optimize the RA enrichment process, the performance and separation characteristics of nine selected macroporous resins with different chemical and physical properties were investigated. SP825 resin was the most effective: the content of RA increased from 0.27% in the original extract to 16.58% in the 50% ethanol fraction (a 61.4-fold increase). During further purification treatment on polyamide resin, 90.23% pure RA could be obtained in the 70% ethanol fraction. RA with a higher purity (>95%) could also be easily obtained using one crystallization operation. The proposed method is simple, easily operated, cost-effective, and environmentally friendly and is suitable for both large-scale RA production and waste management. Copyright © 2013 Elsevier B.V. All rights reserved.

Enantioselective separation of defined endocrine-disrupting nonylphenol isomers.

PubMed

Acir, Ismail-Hakki; Wüst, Matthias; Guenther, Klaus

2016-08-01

Nonylphenol is in the focus of worldwide endocrine-disrupter research and accounted for as a priority hazardous substance of the Water Framework Directive of the European Union. Technical nonylphenol consists of a very complex mixture of isomers and enantiomers. As estrogenic effect and degradation behavior in environmental processes of single nonylphenols are heavily dependent on the structure of the nonyl side chain, it is absolutely necessary to consider the nonylphenol problem from an isomer and enantiomer-specific viewpoint. In this study, an enantiomer-specific separation of eight defined synthesized nonylphenol isomers by five different special chiral cyclodextrin columns was performed underivatized and after methylation, silylation, and acylation. This work demonstrates that three columns out of the investigated five show an excellent separation behavior for the studied different nonylphenol isomers and can be used for the enantiomer-specific determination of nonylphenols in food, other biological matrices, and environmental samples in the future. Graphical abstract Enantiomeric pair of 4-NP170 (4-[1-ethyl-1,3,3-trimethylbutyl]phenol).

Microchip electrospray: improvements in spray and signal stability during gradient elution by an inverted postcolumn makeup flow.

PubMed

Jung, Stephanie; Effelsberg, Uwe; Tallarek, Ulrich

2011-12-01

Dynamic changes in mobile phase composition during high-performance liquid chromatography (HPLC) gradient elution coupled to mass spectrometry (MS) sensitively affect electrospray modes. We investigate the impact of the eluent composition on spray stability and MS response by infusion and injection experiments with a small tetrapeptide in water-acetonitrile mixtures. The employed HPLC/electrospray (ESI)-MS configuration uses a microchip equipped with an enrichment column, a separation column, and a makeup flow (MUF) channel. One nano pump is connected to the separation column, while a second one delivers solvent of exactly inverted composition to the MUF channel. Both solvent streams are united behind the separation column, before the ESI tip, such that the resulting electrosprayed solution always has identical composition during a gradient elution. Analyte peak parameters without and with MUF compensation are determined and discussed with respect to the electrospray mode and eluent composition. The postcolumn MUF significantly improves spray and signal stability over the entire solvent gradient, without compromising the performance of the HPLC separation column. It can also be conveniently implemented on microchip platforms.

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.

Rotating Apparatus for Isoelectric Focusing

NASA Technical Reports Server (NTRS)

Bier, M.

1986-01-01

Remixing of separated fractions prevented. Improved isoelectric focusing apparatus helps to prevent electro-osmosis and convection, both of which cause remixing of separated fractions. Fractionating column segmented and rotated about horizontal axis: Only combined effects of both features fully effective in making good separations. Improved apparatus slowly rotated continuously or rocked (at rotational amplitude of at least 180 degrees) about its horizontal axis so average gravitational vector experienced by fluid is zero and convection is therefore suppressed. Electro-osmosis suppressed and convection further suppressed by separating column into disklike compartments along its length with filters. Experiments have shown dimensions of apparatus not critical. Typical compartment and column volumes are 2 and 40 ml, respectively. Rotation speeds lie between 3 and 30 rpm.

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.

HILIC separation mechanisms of tetracyclines on amino bonded silica column

USDA-ARS?s Scientific Manuscript database

Effects of mobile phase variations on the chromatographic separation on amino bonded silica column in hydrophilic interaction chromatography (HILIC) were investigated for four zwitterionic tetracyclines (TCs): oxytetracycline, doxycycline, chlortetracycline and tetracycline. A mixed-mode retention m...

Chromatographic separation of fructose from date syrup.

PubMed

Al Eid, Salah M

2006-01-01

The objective of this study is to provide a process for separating fructose from a mixture of sugars containing essentially fructose and glucose, obtained from date palm fruits. The extraction procedure of date syrup from fresh dates gave a yield of 86.5% solids after vacuum drying. A process for separating fructose from an aqueous solution of date syrup involved adding the date syrup solutions (20, 30 and 40% by weight) to a chromatographic column filled with Dowex polystyrene strong cation exchange gel matrix resin Ca2 + and divinylbenzene, a functional group, sulfonic acid, particle size 320 microm, with a flow rate of 0.025 and 0.05 bed volume/min, under 30 and 70 degrees C column temperature. After the date sugar solution batch, a calculated quantity of water was added to the column. Glucose was retained by the resin more weakly than fructose and proceeded faster into the water batch flowing ahead. Three fractions were collected: a glucose-rich fraction, a return fraction, and a fructose-rich fraction. The return fraction is based on when the peaks of fructose and glucose were reached, which could be determined by means of an analyzer (polarimeter) based on the property of glucose and fructose solutions to turn the polarization level of polarized light. A high yield of fructose is obtained at 70 degrees C column temperature with a flow rate of 0.025 bed volume/min and date syrup solution containing 40% sugar concentration. The low recovery by weight obtained using date syrup solutions having a sugar concentration of 20 and 30%, encourages the use of a concentration of 40%. However, with the 40% date syrup supply the average concentrations of glucose and fructose in the return fractions were more than 40%, which can be used for diluting the thick date syrup solution extracted from dates.

Neural-network dedicated processor for solving competitive assignment problems

NASA Technical Reports Server (NTRS)

Eberhardt, Silvio P. (Inventor)

1993-01-01

A neural-network processor for solving first-order competitive assignment problems consists of a matrix of N x M processing units, each of which corresponds to the pairing of a first number of elements of (R sub i) with a second number of elements (C sub j), wherein limits of the first number are programmed in row control superneurons, and limits of the second number are programmed in column superneurons as MIN and MAX values. The cost (weight) W sub ij of the pairings is programmed separately into each PU. For each row and column of PU's, a dedicated constraint superneuron insures that the number of active neurons within the associated row or column fall within a specified range. Annealing is provided by gradually increasing the PU gain for each row and column or increasing positive feedback to each PU, the latter being effective to increase hysteresis of each PU or by combining both of these techniques.

Radionuclide Sensors and Systems for Monitoring Technetium-99 and Strontium-90 in Groundwater at the Hanford Site

NASA Astrophysics Data System (ADS)

Grate, J. W.; O'Hara, M. J.; Egorov, O. B.; Burge, S. R.

2009-12-01

We have developed automated sensor and analyzer devices for detection and monitoring of trace radionuclides in water, using preconcentrating columns and radiometric detection. The preconcentrating minicolumn sensor concept combines selective capture and detection in a single functional unit, where the column contains tens to hundreds of milligrams of selectively sorbent material, and the entire column content is monitored with a radiometric detector. Compared to thin film sensors with a few microgram of sorbent, this approach achieves tremendous preconcentration with efficient mass transport via pumping. Furthermore, in an equilibration-based mode of operation, the preconcentration by the sensor is maximized while eliminating the need for consumable reagents to regenerate the column; it can simply be re-equilibrated. We have demonstrated quantification of radionuclides such as technetium-99 to levels below drinking water standards in an equilibration-based process that produces steady state signals, signal proportional to concentration, and easy re-equilibration to new concentration levels. Alternatively, analyzers can be developed with separate separation and detection units that are fluidically linked. We have demonstrated detection of strontium-90 to levels below drinking water standards by this approach. We are developing autonomous systems for at-site monitoring on the Hanford Site in Washington State, using the fluidic sensor and analyzer methods, with the aim of monitoring natural and accelerated attenuation processes, remediation and barrier performance, and contaminant fluxes in the environment. Figure 1. The strontium-90 monitoring method deployed as part of the Burge Environmental Universal Sensor Platform, shown on the shores of the Columbia River on the Hanford site in Washington State.

Automated two-dimensional interface for capillary gas chromatography

DOEpatents

Strunk, M.R.; Bechtold, W.E.

1996-02-20

A multidimensional gas chromatograph (GC) system is disclosed which has wide bore capillary and narrow bore capillary GC columns in series and has a novel system interface. Heart cuts from a high flow rate sample, separated by a wide bore GC column, are collected and directed to a narrow bore GC column with carrier gas injected at a lower flow compatible with a mass spectrometer. A bimodal six-way valve is connected with the wide bore GC column outlet and a bimodal four-way valve is connected with the narrow bore GC column inlet. A trapping and retaining circuit with a cold trap is connected with the six-way valve and a transfer circuit interconnects the two valves. The six-way valve is manipulated between first and second mode positions to collect analyte, and the four-way valve is manipulated between third and fourth mode positions to allow carrier gas to sweep analyte from a deactivated cold trap, through the transfer circuit, and then to the narrow bore GC capillary column for separation and subsequent analysis by a mass spectrometer. Rotary valves have substantially the same bore width as their associated columns to minimize flow irregularities and resulting sample peak deterioration. The rotary valves are heated separately from the GC columns to avoid temperature lag and resulting sample deterioration. 3 figs.

Automated two-dimensional interface for capillary gas chromatography

DOEpatents

Strunk, Michael R.; Bechtold, William E.

1996-02-20

A multidimensional gas chromatograph (GC) system having wide bore capillary and narrow bore capillary GC columns in series and having a novel system interface. Heart cuts from a high flow rate sample, separated by a wide bore GC column, are collected and directed to a narrow bore GC column with carrier gas injected at a lower flow compatible with a mass spectrometer. A bimodal six-way valve is connected with the wide bore GC column outlet and a bimodal four-way valve is connected with the narrow bore GC column inlet. A trapping and retaining circuit with a cold trap is connected with the six-way valve and a transfer circuit interconnects the two valves. The six-way valve is manipulated between first and second mode positions to collect analyte, and the four-way valve is manipulated between third and fourth mode positions to allow carrier gas to sweep analyte from a deactivated cold trap, through the transfer circuit, and then to the narrow bore GC capillary column for separation and subsequent analysis by a mass spectrometer. Rotary valves have substantially the same bore width as their associated columns to minimize flow irregularities and resulting sample peak deterioration. The rotary valves are heated separately from the GC columns to avoid temperature lag and resulting sample deterioration.

Automation of nanoflow liquid chromatography-tandem mass spectrometry for proteome analysis by using a strong cation exchange trap column.

PubMed

Jiang, Xiaogang; Feng, Shun; Tian, Ruijun; Han, Guanghui; Jiang, Xinning; Ye, Mingliang; Zou, Hanfa

2007-02-01

An approach was developed to automate sample introduction for nanoflow LC-MS/MS (microLC-MS/MS) analysis using a strong cation exchange (SCX) trap column. The system consisted of a 100 microm id x 2 cm SCX trap column and a 75 microm id x 12 cm C18 RP analytical column. During the sample loading step, the flow passing through the SCX trap column was directed to waste for loading a large volume of sample at high flow rate. Then the peptides bound on the SCX trap column were eluted onto the RP analytical column by a high salt buffer followed by RP chromatographic separation of the peptides at nanoliter flow rate. It was observed that higher performance of separation could be achieved with the system using SCX trap column than with the system using C18 trap column. The high proteomic coverage using this approach was demonstrated in the analysis of tryptic digest of BSA and yeast cell lysate. In addition, this system was also applied to two-dimensional separation of tryptic digest of human hepatocellular carcinoma cell line SMMC-7721 for large scale proteome analysis. This system was fully automated and required minimum changes on current microLC-MS/MS system. This system represented a promising platform for routine proteome analysis.

Detailed results of ASTP experiment MA-011. [biological processing facility in space

NASA Technical Reports Server (NTRS)

Seaman, G. V. F.; Allen, R. E.; Barlow, G. H.; Bier, M.

1976-01-01

This experiment was developed in order to conduct engineering and operational tests of electrokinetic equipment in a micro-gravity environment. The experimental hardware in general functioned as planned and electrophoretic separations were obtained in space. The results indicated the development of satisfactory sample collection, return, and preservation techniques. The application of a near-zero zeta potential interior wall coating to the experimental columns, confirmation of biocompatibility of all appropriate hardware components, and use of a sterile operating environment provided a significant step forward in the development of a biological processing facility in space. A separation of a test of aldehyde-fixed rabbit, human, and horse red blood cells was obtained. Human kidney cells were separated into several components and viable cells returned to earth. The isotachophoretic separation of red cells was also demonstrated. Problems associated with the hardware led to a lack of success in the attempt to separate subpopulations of human lymphocytes.

Fully automated multifunctional ultrahigh pressure liquid chromatography system for advanced proteome analyses

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

Lee, Jung Hwa; Hyung, Seok-Won; Mun, Dong-Gi

2012-08-03

A multi-functional liquid chromatography system that performs 1-dimensional, 2-dimensional (strong cation exchange/reverse phase liquid chromatography, or SCX/RPLC) separations, and online phosphopeptides enrichment using a single binary nano-flow pump has been developed. With a simple operation of a function selection valve, which is equipped with a SCX column and a TiO2 (titanium dioxide) column, a fully automated selection of three different experiment modes was achieved. Because the current system uses essentially the same solvent flow paths, the same trap column, and the same separation column for reverse-phase separation of 1D, 2D, and online phosphopeptides enrichment experiments, the elution time information obtainedmore » from these experiments is in excellent agreement, which facilitates correlating peptide information from different experiments.« less

Development of Advanced Nuclide Separation and Recovery Methods using Ion-Exchanhge Techniques in Nuclear Backend

NASA Astrophysics Data System (ADS)

Miura, Hitoshi

The development of compact separation and recovery methods using selective ion-exchange techniques is very important for the reprocessing and high-level liquid wastes (HLLWs) treatment in the nuclear backend field. The selective nuclide separation techniques are effective for the volume reduction of wastes and the utilization of valuable nuclides, and expected for the construction of advanced nuclear fuel cycle system and the rationalization of waste treatment. In order to accomplish the selective nuclide separation, the design and synthesis of novel adsorbents are essential for the development of compact and precise separation processes. The present paper deals with the preparation of highly functional and selective hybrid microcapsules enclosing nano-adsorbents in the alginate gel polymer matrices by sol-gel methods, their characterization and the clarification of selective adsorption properties by batch and column methods. The selective separation of Cs, Pd and Re in real HLLW was further accomplished by using novel microcapsules, and an advanced nuclide separation system was proposed by the combination of selective processes using microcapsules.

Separation of polyethylene glycols and amino-terminated polyethylene glycols by high-performance liquid chromatography under near critical conditions.

PubMed

Wei, Y-Z; Zhuo, R-X; Jiang, X-L

2016-05-20

The separation and characterization of polyethylene glycols (PEGs) and amino-substituted derivatives on common silica-based reversed-phase packing columns using isocratic elution is described. This separation is achieved by liquid chromatography under the near critical conditions (LCCC), based on the number of amino functional end groups without obvious effect of molar mass for PEGs. The mobile phase is acetonitrile in water with an optimal ammonium acetate buffer. The separation mechanism of PEG and amino-substituted PEG under the near LCCC on silica-based packing columns is confirmed to be ion-exchange interaction. Under the LCCC of PEG backbone, with fine tune of buffer concentration, the retention factor ratios for benzylamine and phenol in buffered mobile phases, α(benzylamine/phenol)-values, were used to assess the ion-exchange capacity on silica-based reversed-phase packing columns. To the best of our knowledge, this is the first report on separation of amino-functional PEGs independent of the molar mass by isocratic elution using common C18 or phenyl reversed-phase packing columns. Copyright © 2016 Elsevier B.V. All rights reserved.

Reduction of Mn-oxides by ferrous iron in a flow system: column experiment and reactive transport modeling

NASA Astrophysics Data System (ADS)

Postma, D.; Appelo, C. A. J.

2000-04-01

The reduction of Mn-oxide by Fe2+ was studied in column experiments, using a column filled with natural Mn-oxide coated sand. Analysis of the Mn-oxide indicated the presence of both Mn(III) and Mn(IV) in the Mn-oxide. The initial exchange capacity of the column was determined by displacement of adsorbed Ca2+ with Mg2+. Subsequently a FeCl2 solution was injected into the column causing the reduction of the Mn-oxide and the precipitation of Fe(OH)3. Finally the exchange capacity of the column containing newly formed Fe(OH)3 was determined by injection of a KBr solution. During injection of the FeCl2 solution into the column, an ion distribution pattern was observed in the effluent that suggests the formation of separate reaction fronts for Mn(III)-oxide and Mn(IV)-oxide travelling at different velocities through the column. At the proximal reaction front, Fe2+ reacts with MnO2 producing Fe(OH)3, Mn2+ and H+. The protons are transported downstream and cause the disproportionation of MnOOH at a separate reaction front. Between the two Mn reaction fronts, the dissolution and precipitation of Fe(OH)3 and Al(OH)3 act as proton buffers. Reactive transport modeling, using the code PHREEQC 2.0, was done to quantify and analyze the reaction controls and the coupling between transport and chemical processes. A model containing only mineral equilibria constraints for birnessite, manganite, gibbsite, and ferrihydrite, was able to explain the overall reaction pattern with the sequential appearance of Mn2+, Al3+, Fe3+, and Fe2+ in the column outlet solution. However, the initial breakthrough of a peak of Ca2+ and the observed pH buffering indicated that exchange processes were of importance as well. The amount of potential exchangers, such as birnessite and ferrihydrite, did vary in the course of the experiment. A model containing surface complexation coupled to varying concentrations of birnessite and ferrihydrite and a constant charge exchanger in addition to mineral equilibria provided a satisfactory description of the distribution of all solutes in time and space. However, the observed concentration profiles are more gradual than indicated by the equilibrium model. Reaction kinetics for the dissolution of MnO2 and MnOOH and dissolution of Al(OH)3 were incorporated in the model, which explained the shape of the breakthrough curves satisfactorily. The results of this study emphasize the importance of understanding the interplay between chemical reactions and transport in addition to interactions between redox, proton buffering, and adsorption processes when dealing with natural sediments. Reactive transport modeling is a powerful tool to analyze and quantify such interactions.

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.

Post-synthetic modification of MIL-101(Cr) with pyridine for high-performance liquid chromatographic separation of tocopherols.

PubMed

Yang, Fang; Yang, Cheng-Xiong; Yan, Xiu-Ping

2015-05-01

Effective separation of tocopherols is challenging and significant due to their structural similarity and important biological role. Here we report the post-synthetic modification of metal-organic framework (MOF) MIL-101(Cr) with pyridine for high-performance liquid chromatographic (HPLC) separation of tocopherols. Baseline separation of four tocopherols was achieved on a pyridine-grafted MIL-101(Cr) packed column within 10 min using hexane/isopropanol (96:4, v/v) as the mobile phase at a flow rate of 0.5 mL min(-1). The pyridine-grafted MIL-101(Cr) packed column gave high column efficiency (85,000 plates m(-1) for δ-tocopherol) and good precision (0.2-0.3% for retention time, 1.8-3.4% for peak area, 2.6-2.7% for peak height), and also offered much better performance than unmodified MIL-101(Cr) and commercial amino-bonded silica packed column for HPLC separation of tocopherols. The results not only show the promising application of pyridine-grafted MIL-101(Cr) as a novel stationary phase for HPLC separation of tocopherols, but also reveal a facile post-modification of MOFs to expand the application of MOFs in separation sciences. Copyright © 2015 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.

Fiber-based monolithic columns for liquid chromatography.

PubMed

Ladisch, Michael; Zhang, Leyu

2016-10-01

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

Liquid Crystals in Chromatography

NASA Astrophysics Data System (ADS)

Witkiewicz, Zygfryd

The following sections are included: * INTRODUCTION * LIQUID CRYSTALS SUITABLE FOR GAS CHROMATOGRAPHY * Monomeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Conventional Analytical Columns * Capillary Columns * FACTORS AFFECTING THE CHROMATOGRAPHIC SEPARATIONS ON LIQUID CRYSTAL STATIONARY PHASES * Kind of Mesophase of the Liquid Crystal * Molecular Structure of the Liquid Crystals and of the Chromatographed Substances * Substrate on which the Liquid Crystal is Deposited * ANALYTICAL APPLICATIONS OF LIQUID CRYSTAL STATIONARY PHASES IN GAS CHROMATOGRAPHY * Separation of Isomers of Benzene and Naphthalene Derivatives * Separation of Alkane and Alkene Isomers * Separation of Mixtures of Benzene and Aliphatic Hydrocarbon Derivatives Containing Heteroatoms * Separation of Polynuclear Hydrocarbons * INVESTIGATION OF THE PROPERTIES OF LIQUID CRYSTALS BY GAS CHROMATOGRAPHY * APPLICATION OF LIQUID CRYSTALS IN LIQUID CHROMATOGRAPHY * Column Chromatography * Thin-Layer Chromatography * APPLICATION OF LIQUID CRYSTAL STATIONARY PHASES IN SUPERCRITICAL FLUID CHROMATOGRAPHY * FINAL REMARKS * References

Final summarizing report on Grant DE-SC0001014 "Separation of Highly Complex Mixtures by Two-dimension Liquid Chromatography"

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

Guiochon, Georges

The goal of our research was a fundamental investigation of methods available for the coupling of two separate chromatographic separations that would considerably enhance the individual separation power of each of these two separations. This gain arises from the combination of two independent retention mechanisms, one of them separating the components that coelute on the other column, making possible the separation of many more compounds in a given time. The two separation mechanisms used must be very different. This is possible because many retention mechanisms are available, using different kinds of molecular interactions, hydrophobic or hydrophilic interactions, polar interactions, hydrogenmore » bonding, complex formation, ionic interactions, steric exclusion. Two methods can be used, allowing separations to be performed in space (spreading the bands of sample components on a plate covered with stationary phase layer) or in time (eluting the sample components through a column and detecting the bands leaving the column). Both offer a wide variety of possible combinations and were studied.« less

Gas chromatographic separation of fatty acid methyl esters on weakly polar capillary columns.

PubMed

Yamamoto, Kouhei; Kinoshita, Akemi; Shibahara, Akira

2008-02-22

It was found that weakly polar columns, routinely used in capillary GC for analyzing sterols, food additives, etc., can also be used for separating fatty acid methyl esters (FAMEs). On these columns, FAMEs elute in the order of their unsaturation. The equivalent chain-length value of methyl 22:6 is below 23.00. This means FAMEs within a carbon chain length, having up to six double bonds, elute before the next (one carbon longer) saturated FAME elutes. Peak identification is easy. Weakly polar columns are compatible in both GC and GC/MS systems.

Hormone Purification by Isoelectric Focusing

NASA Technical Reports Server (NTRS)

Bier, M.

1985-01-01

Various ground-based research approaches are being applied to a more definitive evaluation of the natures and degrees of electroosmosis effects on the separation capabilities of the Isoelectric Focusing (IEF) process. A primary instrumental system for this work involves rotationally stabilized, horizontal electrophoretic columns specially adapted for the IEF process. Representative adaptations include segmentation, baffles/screens, and surface coatings. Comparative performance and development testing are pursued against the type of column or cell established as an engineering model. Previously developed computer simulation capabilities are used to predict low-gravity behavior patterns and performance for IEF apparatus geometries of direct project interest. Three existing mathematical models plus potential new routines for particular aspects of simulating instrument fluid patterns with varied wall electroosmosis influences are being exercised.

Fast comprehensive two-dimensional gas chromatography method for fatty acid methyl ester separation and quantification using dual ionic liquid columns.

PubMed

Nosheen, Asia; Mitrevski, Blagoj; Bano, Asghari; Marriott, Philip J

2013-10-18

Safflower oil is a complex mixture of C18 saturated and unsaturated fatty acids amongst other fatty acids, and achieving separation between these similar structure components using one dimensional gas chromatography (GC) may be difficult. This investigation aims to obtain improved separation of fatty acid methyl esters in safflower oil, and their quantification using comprehensive two-dimensional GC (GC×GC). Here, GC×GC separation is accomplished by the coupling of two ionic liquid (IL) column phases: the combination of SLB-IL111 with IL59 column phases was finally selected since it provided excellent separation of a FAME standard mixture, as well as fatty acids in safflower and linseed oil, compared to other tested column sets. Safflower oil FAME were well separated in a short run of 16min. FAME validation was demonstrated by method reproducibility, linearity over a range up to 500mgL(-1), and limits of detection which ranged from 1.9mgL(-1) to 5.2mgL(-1) at a split ratio of 20:1. Quantification was carried out using two dilution levels of 200-fold for major components and 20-fold for trace components. The fatty acids C15:0 and C17:0 were not reported previously in safflower oil. The SLB-IL111/IL59 column set proved to be an effective and novel configuration for separation and quantification of vegetable and animal oil fatty acids. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

PubMed

Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

2015-07-01

Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Large-scale single-chirality separation of single-wall carbon nanotubes by simple gel chromatography

PubMed Central

Liu, Huaping; Nishide, Daisuke; Tanaka, Takeshi; Kataura, Hiromichi

2011-01-01

Monostructured single-wall carbon nanotubes (SWCNTs) are important in both scientific research and electronic and biomedical applications; however, the bulk separation of SWCNTs into populations of single-chirality nanotubes remains challenging. Here we report a simple and effective method for the large-scale chirality separation of SWCNTs using a single-surfactant multicolumn gel chromatography method utilizing one surfactant and a series of vertically connected gel columns. This method is based on the structure-dependent interaction strength of SWCNTs with an allyl dextran-based gel. Overloading an SWCNT dispersion on the top column results in the adsorption sites of the column becoming fully occupied by the nanotubes that exhibit the strongest interaction with the gel. The unbound nanotubes flow through to the next column, and the nanotubes with the second strongest interaction with the gel are adsorbed in this stage. In this manner, 13 different (n, m) species were separated. Metallic SWCNTs were finally collected as unbound nanotubes because they exhibited the lowest interaction with the gel. PMID:21556063

Iptycene-based stationary phase with three-dimensional aromatic structure for highly selective separation of H-bonding analytes and aromatic isomers.

PubMed

Yang, Xiaohong; Han, Ying; Qi, Meiling; Chen, Chuanfeng

2016-05-06

Unique structures and molecular recognition ability endow iptycene derivatives with great potential as stationary phases in chromatography, which, however, has not been explored yet. Herein, we report the first example of utilizing a pentiptycene quinone (PQ) for gas chromatographic (GC) separations. Remarkably, the statically coated capillary column with the stationary phase achieved extremely high column efficiency of 4800 plates/m. It exhibited preferential retention and high resolving capability for H-bonding and aromatic analytes and positional isomers, showing advantages over the ordinary polysiloxane phase. Moreover, the fabricated iptycene column showed excellent separation repeatability with RSD values of 0.02-0.06% for intra-day, 0.20-0.35% for inter-day and 3.1-5.5% for between-column, respectively. In conclusion, iptycene derivatives as a new class of stationary phases show promising future for their use in GC separations. Copyright © 2016 Elsevier B.V. All rights reserved.

GOBF-ARMA based model predictive control for an ideal reactive distillation column.

PubMed

Seban, Lalu; Kirubakaran, V; Roy, B K; Radhakrishnan, T K

2015-11-01

This paper discusses the control of an ideal reactive distillation column (RDC) using model predictive control (MPC) based on a combination of deterministic generalized orthonormal basis filter (GOBF) and stochastic autoregressive moving average (ARMA) models. Reactive distillation (RD) integrates reaction and distillation in a single process resulting in process and energy integration promoting green chemistry principles. Improved selectivity of products, increased conversion, better utilization and control of reaction heat, scope for difficult separations and the avoidance of azeotropes are some of the advantages that reactive distillation offers over conventional technique of distillation column after reactor. The introduction of an in situ separation in the reaction zone leads to complex interactions between vapor-liquid equilibrium, mass transfer rates, diffusion and chemical kinetics. RD with its high order and nonlinear dynamics, and multiple steady states is a good candidate for testing and verification of new control schemes. Here a combination of GOBF-ARMA models is used to catch and represent the dynamics of the RDC. This GOBF-ARMA model is then used to design an MPC scheme for the control of product purity of RDC under different operating constraints and conditions. The performance of proposed modeling and control using GOBF-ARMA based MPC is simulated and analyzed. The proposed controller is found to perform satisfactorily for reference tracking and disturbance rejection in RDC. Copyright © 2015 Elsevier Inc. All rights reserved.

Ionic liquids as stationary phases for fatty acid analysis by gas chromatography.

PubMed

Fanali, C; Micalizzi, G; Dugo, P; Mondello, L

2017-12-04

The present paper provides an overview of the application of ionic liquid (IL) columns for GC analysis of fatty acid methyl esters (FAMEs). Although their separation can be carried out utilizing GC columns containing polar stationary phases, some ILs have been employed as stationary phases, either commercial or laboratory made, in GC analysis. Monodimensional and bidimensional GC methods have been optimized in order to achieve the best separation especially considering the geometric and positional isomers of unsaturated fatty acids. Several methods for the analysis of trans-fatty acids have also been reported. The use of GC-GC, using either the same IL columns or different columns in the first and second dimensions, allowed the separation of a large number of FAMEs. The application of the IL columns for GC analysis of FAMEs in different types of real samples is described, e.g., oil of different nature (fish, flaxseed, and olive), margarine and butter, biodiesel, milk, bacteria etc.

Dopamine-imprinted monolithic column for capillary electrochromatography.

PubMed

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

2017-11-01

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

Shell and small particles; evaluation of new column technology.

PubMed

Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2009-01-15

The performance of 5 cm long columns packed with shell particles was compared to totally porous sub-2 microm particles in gradient and isocratic elution separations of hormones (dienogest, finasteride, gestodene, levonorgestrel, estradiol, ethinylestradiol, noretistherone acetate, bicalutamide and tibolone). Peak capacities around 140-150 could be achieved in 25 min with the 5 cm long columns. The Ascentis Express column (packed with 2.7 microm shell particles) showed similar efficiency to sub-2 microm particles under gradient conditions. Applying isocratic separation, the column of 2.7 microm shell particles had a reduced plate height minimum of approximately h=1.6. It was much smaller than obtained with totally porous particles (h approximately = 2.8). The impedance time also proved more favorable with 2.7 microm shell particles than with totally porous particles. The influence of extra-column volume on column efficiency was investigated. The extra-column dispersion of the chromatographic system may cause a shift of the HETP curves.

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.

Liquid-phase thermal diffusion isotope separation apparatus and method having tapered column

DOEpatents

Rutherford, William M.

1988-05-24

A thermal diffusion counterflow method and apparatus for separating isotopes in solution in which the solution is confined in a long, narrow, vertical slit which tapers from bottom to top. The variation in the width of the slit permits maintenance of a stable concentration distribution with relatively long columns, thus permitting isotopic separation superior to that obtainable in the prior art.

Liquid-phase thermal diffusion isotope separation apparatus and method having tapered column

DOEpatents

Rutherford, W.M.

1985-12-04

A thermal diffusion counterflow method and apparatus for separating isotopes in solution in which the solution is confined in a long, narrow, vertical slit which tapers from bottom to top. The variation in the width of the slit permits maintenance of a stable concentration distribution with relatively long columns, thus permitting isotopic separation superior to that obtained in the prior art.

Separation of the Components of a Commercial Analgesic Tablet: A Two-Week Sequence Comparing Purification by Two-Base Extraction and Column Chromatography

ERIC Educational Resources Information Center

Revell, Kevin D.

2011-01-01

A new laboratory experiment is described in which students compare two benchtop separation methods to isolate the three active components of the commercial analgesic Excedrin. In the two-week sequence, aspirin, acetaminophen, and caffeine are separated using either a two-base liquid-liquid extraction or silica column chromatography. Students then…

Separation of fatty acid methyl esters by GC-online hydrogenation × GC.

PubMed

Delmonte, Pierluigi; Fardin-Kia, Ali Reza; Rader, Jeanne I

2013-02-05

The separation of fatty acid methyl esters (FAME) provided by a 200 m × 0.25 mm SLB-IL111 capillary column is enhanced by adding a second dimension of separation ((2)D) in a GC × GC design. Rather than employing two GC columns of different polarities or using different elution temperatures, the separation in the two-dimensional space is achieved by altering the chemical structure of selected analytes between the two dimensions of separation. A capillary tube coated with palladium is added between the first dimension of separation ((1)D) column and the cryogenic modulator, providing the reduction of unsaturated FAMEs to their fully saturated forms. The (2)D separation is achieved using a 2.5 m × 0.10 mm SLB-IL111 capillary column and separates FAMEs based solely on their carbon skeleton. The two-dimensional separation can be easily interpreted based on the principle that all the saturated FAMEs lie on a straight diagonal line bisecting the separation plane, while the FAMEs with the same carbon skeleton but differing in the number, geometric configuration or position of double bonds lie on lines parallel to the (1)D time axis. This technique allows the separation of trans fatty acids (FAs) and polyunsaturated FAs (PUFAs) in a single experiment and eliminates the overlap between PUFAs with different chain lengths. To our knowledge, this the first example of GC × GC in which a chemical change is instituted between the two dimensions to alter the relative retentions of components and identify unsaturated FAMEs.

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.

The separation of flavonoids from Pongamia pinnata using combination columns in high-speed counter-current chromatography with a three-phase solvent system.

PubMed

Yin, Hao; Zhang, Si; Long, Lijuan; Yin, Hang; Tian, Xinpeng; Luo, Xiongming; Nan, Haihan; He, Sha

2013-11-08

The mangrove plant Pongamia pinnata (Leguminosae) is well known as a plant pesticide. Previous studies have indicated that the flavonoids are responsible of the biological activities of the plant. A new high-speed counter-current chromatography (HSCCC) method for the separation of three flavonoids, karanjin (1), pinnatin (2), and pongaflavone (3), from P. pinnata was developed in the present study. The lower and intermediate phase (LP and IP) of a new three-phase solvent system, n-hexane-acetonitrile-dichloromethane-water, at a volume ratio of 5:5:1:5, were used as the stationary phases, while the upper phase (UP) was used as the mobile phase, and the volume ratio between the stationary phases in the CCC column could be tuned by varying the initial pumped volume ratio of the stationary phases. The CCC columns containing all three phases of the solvent system were considered combination columns. According to the theories of combination column, it is possible to optimize the retention time of the target compounds by varying the volume ratio of the stationary phases in the HSCCC combination columns, as well as the suitable volume ratios of the stationary phases for the separation of the target compounds were predicted from the partition coefficients of the compounds in the three-phase solvent system. Then, three HSCCC separations using the combination columns with initial pumped LP:IP volume ratios of 1:0, 0.9:0.1, and 0.7:0.3 were performed separately based on the prediction. Three target compounds were prepared with high purity when the initial pumped volume ratio of the stationary phases was 0.9:0.1. The baseline separation of compounds 2 and 3 was achieved on the combination column with an initial pumped volume ratio of 0.7:0.3. Furthermore, the three experiments clearly demonstrated that the retentions and resolutions of the target compounds increased with an increasing volume ratio of IP, which is consistent with the prediction for the retention times for the solutes on combination columns. The method proposed here reduces the need for solvent selection compared with the conventional method and may have broad potential applicability in the preparation of natural products. Copyright © 2013 Elsevier B.V. All rights reserved.

Atmospheric processes affecting the separation of volcanic ash and SO2 in volcanic eruptions: inferences from the May 2011 Grímsvötn eruption

NASA Astrophysics Data System (ADS)

Prata, Fred; Woodhouse, Mark; Huppert, Herbert E.; Prata, Andrew; Thordarson, Thor; Carn, Simon

2017-09-01

The separation of volcanic ash and sulfur dioxide (SO2) gas is sometimes observed during volcanic eruptions. The exact conditions under which separation occurs are not fully understood but the phenomenon is of importance because of the effects volcanic emissions have on aviation, on the environment, and on the earth's radiation balance. The eruption of Grímsvötn, a subglacial volcano under the Vatnajökull glacier in Iceland during 21-28 May 2011 produced one of the most spectacular examples of ash and SO2 separation, which led to errors in the forecasting of ash in the atmosphere over northern Europe. Satellite data from several sources coupled with meteorological wind data and photographic evidence suggest that the eruption column was unable to sustain itself, resulting in a large deposition of ash, which left a low-level ash-rich atmospheric plume moving southwards and then eastwards towards the southern Scandinavian coast and a high-level predominantly SO2 plume travelling northwards and then spreading eastwards and westwards. Here we provide observational and modelling perspectives on the separation of ash and SO2 and present quantitative estimates of the masses of ash and SO2 that erupted, the directions of transport, and the likely impacts. We hypothesise that a partial column collapse or sloughing fed with ash from pyroclastic density currents (PDCs) occurred during the early stage of the eruption, leading to an ash-laden gravity intrusion that was swept southwards, separated from the main column. Our model suggests that water-mediated aggregation caused enhanced ash removal because of the plentiful supply of source water from melted glacial ice and from entrained atmospheric water. The analysis also suggests that ash and SO2 should be treated with separate source terms, leading to improvements in forecasting the movement of both types of emissions.

Column Selection for Biomedical Analysis Supported by Column Classification Based on Four Test Parameters

PubMed Central

Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

2016-01-01

This article focuses on correlating the column classification obtained from the method created at the Katholieke Universiteit Leuven (KUL), with the chromatographic resolution attained in biomedical separation. In the KUL system, each column is described with four parameters, which enables estimation of the FKUL value characterising similarity of those parameters to the selected reference stationary phase. Thus, a ranking list based on the FKUL value can be calculated for the chosen reference column, then correlated with the results of the column performance test. In this study, the column performance test was based on analysis of moclobemide and its two metabolites in human plasma by liquid chromatography (LC), using 18 columns. The comparative study was performed using traditional correlation of the FKUL values with the retention parameters of the analytes describing the column performance test. In order to deepen the comparative assessment of both data sets, factor analysis (FA) was also used. The obtained results indicated that the stationary phase classes, closely related according to the KUL method, yielded comparable separation for the target substances. Therefore, the column ranking system based on the FKUL-values could be considered supportive in the choice of the appropriate column for biomedical analysis. PMID:26805819

Column Selection for Biomedical Analysis Supported by Column Classification Based on Four Test Parameters.

PubMed

Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

2016-01-21

This article focuses on correlating the column classification obtained from the method created at the Katholieke Universiteit Leuven (KUL), with the chromatographic resolution attained in biomedical separation. In the KUL system, each column is described with four parameters, which enables estimation of the FKUL value characterising similarity of those parameters to the selected reference stationary phase. Thus, a ranking list based on the FKUL value can be calculated for the chosen reference column, then correlated with the results of the column performance test. In this study, the column performance test was based on analysis of moclobemide and its two metabolites in human plasma by liquid chromatography (LC), using 18 columns. The comparative study was performed using traditional correlation of the FKUL values with the retention parameters of the analytes describing the column performance test. In order to deepen the comparative assessment of both data sets, factor analysis (FA) was also used. The obtained results indicated that the stationary phase classes, closely related according to the KUL method, yielded comparable separation for the target substances. Therefore, the column ranking system based on the FKUL-values could be considered supportive in the choice of the appropriate column for biomedical analysis.

Separation science is the key to successful biopharmaceuticals.

PubMed

Guiochon, Georges; Beaver, Lois Ann

2011-12-09

The impact of economic change, advances in science, therapy and production processes resulted in considerable growth in the area of biopharmaceuticals. Progress in selection of microorganisms and improvements in cell culture and bioreactors is evidenced by increased yields of the desired products in the complex fermentation mixture. At this stage the downstream process of extraction and purification of the desired biopharmaceutical requires considerable attention in the design and operation of the units used for preparative chromatography. Understanding of the process, optimization of column design and experimental conditions have become critical to the biopharmaceutical industry in order to minimize production costs while satisfying new regulatory requirements. Optimization of the purification of biopharmaceuticals by preparative liquid chromatography including an examination of column preparation and bed properties is the focus of this manuscript. Copyright © 2011 Elsevier B.V. All rights reserved.

Instrument for the measurement and determination of chemical pulse column parameters

DOEpatents

Marchant, Norman J.; Morgan, John P.

1990-01-01

An instrument for monitoring and measuring pneumatic driving force pulse parameters applied to chemical separation pulse columns obtains real time pulse frequency and root mean square amplitude values, calculates column inch values and compares these values against preset limits to alert column operators to the variations of pulse column operational parameters beyond desired limits.

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2011 CFR

2011-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2013 CFR

2013-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2014 CFR

2014-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

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.

Influence of the Kinetics of Heat and Mass Transfer in a Binary-Rectification Column on the Realizability Range of its Regimes

NASA Astrophysics Data System (ADS)

Zaeva, M. A.; Tsirlin, A. M.; Sukin, I. A.

2018-05-01

The range of realizable rates of flows in a binary-rectification column in which heat is supplied into the boiler and is removed from the dephlegmator was investigated. It is shown that this range is determined by two characteristic parameters related to the kinetics of heat and mass transfer in the column and the composition of the mixture subjected to separation. The limiting capabilities of a cascade of two binary-rectification columns for the separation of a ternary mixture in it were considered. The conditions for an optimum sequence of separation of a mixture in this cascade and for a consistent arrangement of its heat and mass exchange surfaces and the relation between the ultimate production rate of the cascade and the total heat losses in it were determined.

Influence of the Kinetics of Heat and Mass Transfer in a Binary-Rectification Column on the Realizability Range of its Regimes

NASA Astrophysics Data System (ADS)

Zaeva, M. A.; Tsirlin, A. M.; Sukin, I. A.

2018-03-01

The range of realizable rates of flows in a binary-rectification column in which heat is supplied into the boiler and is removed from the dephlegmator was investigated. It is shown that this range is determined by two characteristic parameters related to the kinetics of heat and mass transfer in the column and the composition of the mixture subjected to separation. The limiting capabilities of a cascade of two binary-rectification columns for the separation of a ternary mixture in it were considered. The conditions for an optimum sequence of separation of a mixture in this cascade and for a consistent arrangement of its heat and mass exchange surfaces and the relation between the ultimate production rate of the cascade and the total heat losses in it were determined.

Determination of strontium-90 in milk samples using a controlled precipitation clean-up step prior to ion-chromatography.

PubMed

Cobb, J; Warwick, P; Carpenter, R C; Morrison, R T

1995-12-01

Strontium-90 may be determined by beta-counting its yttrium-90 daughter following separation by ion-chromatography, using a three column system comprising a chelating concentrator column, a cation-exchange column and an anion-exchange separator column. The column system has previously been applied to the determination of strontium-90 in water and urine samples. The applicability of the system to the analysis of milk is hampered by the large concentrations of calcium present, which significantly reduces the extraction of yttrium-90 by the concentrator column. A maximum of approximately 200 mg of calcium can be present for the successful extraction of yttrium-90, which greatly limits the quantity of milk that can be analysed. The quantity of milk analysed can be increased by the inclusion of a controlled precipitation step prior to the ion-chromatographic separation. The precipitation is carried out on acid digested milk samples by the addition of ammonia solution until the addition of one drop causes a reduction in pH resulting in the precipitation of calcium hydrogenphosphate. Under these conditions, approximately 20% of the calcium present in the original milk sample is precipitated, yttrium-90 is precipitated whereas strontium-90 is not precipitated. Dissolution of the precipitate, followed by separation of yttrium-90 using the ion-chromatography system facilitates the analysis of a litre of milk with recoveries of greater than 80%.

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.

Development of a GMP Phase III purification process for VB4-845, an immunotoxin expressed in E. coli using high cell density fermentation.

PubMed

Premsukh, Arjune; Lavoie, Joelle M; Cizeau, Jeannick; Entwistle, Joycelyn; MacDonald, Glen C

2011-07-01

VB4-845 is a recombinant immunotoxin comprised of an anti-epithelial cell adhesion molecule (EpCAM) scFv fused to a truncated form of the bacterial toxin, Pseudomonas exotoxin A. VB4-845, purified from TB fed-batch fermentation, showed clinical efficacy when administered locally to treat non-muscle invasive bladder cancer (NMIBC) and squamous cell carcinomas of the head and neck (SCCHN). Here, we describe the implementation of an Escherichia coli high cell density (HCD) cultivation and purification process for VB4-845. HCD cultivation was a prerequisite for achieving higher yields necessary for Phase III clinical trials and commercialization. Using this process, the VB4-845 titer in the supernatant was increased by 30-fold over the original TB fed-batch cultivation. To obtain clinical grade material, a process involving a five-step column purification procedure was implemented and led to an overall recovery of ∼ 40%. VB4-845 purity of >97% was achieved after the first three columns following the removal of low-molecular weight product-related impurities and aggregates. Endotoxins were effectively separated from VB4-845 on the Q-columns and by washing the Ni-column with a detergent buffer while host cell proteins were removed using ceramic hydroxyapatite. Comparability studies demonstrated that the purified product from the Phase III process was identical to the Phase II reference standard produced using TB fed-batch fermentation. Copyright © 2011 Elsevier Inc. All rights reserved.

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

Adams, W.D.

Passive solar heating was used in a still in which a packed column packed with popped popcorn separates the alcohol and water vapors. The still's performance was not satisfactory, and it is concluded that passive solar heating could have been better used to preheat makeup water for the fermentation process and to maintain proper fermentation temperatures during the winter. (LEW)

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

Blay, J.A.

The problem of the determination of micro-amounts of uranium in aqueous and organic phases in liquid-liquid extraction processes, original ones, and extraction residues was solved by a chromatographic separation of the uranium by means of columns of activated cellulose and further spectrophotometric evaluation using the thiocyanate complex in aqueous medium. The usable range is 5 to 200 mu g.

TESTING SOLIDS SETTING APPARATUSES FOR DESIGN AND OPERATION OF WET-WEATHER FLOW SOLIDS-LIQUID SEPARATION PROCESSES

EPA Science Inventory

This study was a side-by-side comparison of two settling evaluation methods: one traditional and one new. The project investigated whether these column tests were capable of capturing or representing the rapidly settling particles present in wet-weather flows (WWF). The report r...

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.

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

PubMed

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

2017-05-19

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

Separation of polychlorinated biphenyls by fast gas chromatography.

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

Alvarado, J. S.; Silzer, J.; Lemley, F.

1997-12-01

The separation of commercially available polychlorinated biphenyls (PCBs) by fast gas chromatography (fast GC) has been studied. Aroclor 1254 was separated by using two column types: DB-1 and SPB-608. The fast GC used a split-splitless injector to introduce the sample, followed by a cold trap at -90 C to focus the sample. Rapid heating was used to introduce the sample into the short chromatographic column to decrease band broadening. Hydrogen was the carrier gas at velocities of 100 to 125 cm s-1. Analyses were performed by using an electron capture detector (ECD). Separation was achieved with both columns in lessmore » than 6 min. With the greatly shortened run times, reproducibility can be tested quickly and consequently with low cost.« less

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%.

SEPARATION OF T-MAZ ETHOXYLATED SORBITAN FATTY ACID ESTERS BY SUPERCRITICAL FLUID CHROMATOGRAPHY

EPA Science Inventory

The application of supercritical fluid chromatography (SFC) to the analysis of T-MAZ ethoxylated sorbitan fatty acid esters is described. FC separation methods utilize a density programming technique and a 50 um I.D. capillary column. his work demonstrates that capillary column S...

Chiral separation of G-type chemical warfare nerve agents via analytical supercritical fluid chromatography.

PubMed

Kasten, Shane A; Zulli, Steven; Jones, Jonathan L; Dephillipo, Thomas; Cerasoli, Douglas M

2014-12-01

Chemical warfare nerve agents (CWNAs) are extremely toxic organophosphorus compounds that contain a chiral phosphorus center. Undirected synthesis of G-type CWNAs produces stereoisomers of tabun, sarin, soman, and cyclosarin (GA, GB, GD, and GF, respectively). Analytical-scale methods were developed using a supercritical fluid chromatography (SFC) system in tandem with a mass spectrometer for the separation, quantitation, and isolation of individual stereoisomers of GA, GB, GD, and GF. Screening various chiral stationary phases (CSPs) for the capacity to provide full baseline separation of the CWNAs revealed that a Regis WhelkO1 (SS) column was capable of separating the enantiomers of GA, GB, and GF, with elution of the P(+) enantiomer preceding elution of the corresponding P(-) enantiomer; two WhelkO1 (SS) columns had to be connected in series to achieve complete baseline resolution. The four diastereomers of GD were also resolved using two tandem WhelkO1 (SS) columns, with complete baseline separation of the two P(+) epimers. A single WhelkO1 (RR) column with inverse stereochemistry resulted in baseline separation of the GD P(-) epimers. The analytical methods described can be scaled to allow isolation of individual stereoisomers to assist in screening and development of countermeasures to organophosphorus nerve agents. © 2014 The Authors. Chirality published by John Wiley Periodicals, Inc.

Chiral separation of isoxanthohumol and 8-prenylnaringenin in beer, hop pellets, and hops by HPLC with chiral columns.

PubMed

Moriya, Hyuga; Tanaka, Sohei; Iida, Yukari; Kitagawa, Satomi; Aizawa, Sen-Ichi; Taga, Atsushi; Terashima, Hiroyuki; Yamamoto, Atsushi; Kodama, Shuji

2018-05-16

Xanthohumol, isoxanthohumol, and 8-prenylnaringenin in beer, hop, and hop pellet samples were analyzed by HPLC using InertSustain phenyl column and the mobile phase containing 40% methanol and 12% 2-propanol. Fractions of isoxanthohumol and 8-prenylnaringenin obtained by the above HPLC were separately collected. Isoxanthohumol and 8-prenylnaringenin were enantioseparated by HPLC using Chiralcel OD-H column with a mobile phase composed of hexane/ethanol (90/10, v/v) and Chiralpak AD-RH column with a mobile phase composed of methanol/2-propanol/water (40/20/40, v/v/v), respectively. Both of isoxanthohumol and 8-prenylnaringenin from beer, hop, and hop pellet samples were found to be a racemic mixture. This can be explained that the two analytes were produced by non-enzymatic process. The effects of boiling conditions on the conversion of xanthohumol into isoxanthohumol were also studied. A higher concentration of ethanol in heating solvent resulted in a decrease in the conversion ratio and the conversion was stopped by addition of ethanol more than 50% (v/v). The isomerization was significantly affected pH (2-10) and the boiling medium at pH 5 was minimum for the conversion. Therefore, it was suggested that xanthohumol was relatively difficult to convert to isoxanthohumol in wort (pH 5-5.5) during boiling. This article is protected by copyright. All rights reserved.

[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.

Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

PubMed

Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

2017-09-01

A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2011-01-01

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

Preparation 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.

Isolation of biofunctional bovine immunoglobulin G from milk- and colostral whey with mixed-mode chromatography at lab and pilot scale.

PubMed

Heidebrecht, Hans-Jürgen; Kainz, Bernadette; Schopf, Roland; Godl, Klaus; Karcier, Züleyha; Kulozik, Ulrich; Förster, Beatrix

2018-05-23

The aim of the present work was to develop a new scalable and cost-efficient process to isolate bovine immunoglobulin G from colostral whey with high purity and minimal loss of activity. The mixed mode material Mercapto-Ethyl-Pyridine-Hypercel™ was identified appropriate for direct capture of immunoglobulin G. The binding mechanism is primarily based on hydrophobic interactions at physiological conditions. As compared to immunoglobulin G, all other low molecular whey proteins such as α-Lactalbumin or β-Lactoglobulin, except lactoperoxidase, are more hydrophilic and were therefore found in the flow-through fraction. In order to remove lactoperoxidase as an impurity the column was combined in series with a second mixed mode material (Capto™- with N-benzoyl-homocysteine as ligand) using the same binding conditions. At pH 7.5 the carboxyl group of this ligand is negatively charged and can hence bind the positively charged lactoperoxidase, whose isoelectric point is at pH 9.6. After sample application, the columns were eluted separately. By combining the two columns it was possible to obtain immunoglobulin G with a purity of >96.1% and yield of 65-80%. The process development was carried out using 1 mL columns and upscaling was performed in three steps up to a column volume of 8800 mL for the Hypercel™ column and 3000 mL for the Capto™- column. At this scale it is possible to obtain 130-150 g pure immunoglobulin G from 3 L colostrum within five hours, including the regeneration of both columns. Additionally, the impact of freeze-drying on the isolated immunoglobulin G was studied. The nativity of the freeze dried immunoglobulin was above 95%, which was proven by reversed phase liquid chromatography and validated by differential scanning calorimetry. The activity of immunoglobulin G was preserved over the isolation process and during drying as measured by enzyme-linked immunosorbent assay. In conclusion, by applying the proposed isolation process, it becomes feasible to obtain pure, active and stable imunnunoglobulin G at large scale. Copyright © 2018 Elsevier B.V. All rights reserved.

High‐precision determination of lithium and magnesium isotopes utilising single column separation and multi‐collector inductively coupled plasma mass spectrometry

PubMed Central

Misra, Sambuddha; Lloyd, Nicholas; Elderfield, Henry; Bickle, Mike J.

2017-01-01

Rationale Li and Mg isotopes are increasingly used as a combined tool within the geosciences. However, established methods require separate sample purification protocols utilising several column separation procedures. This study presents a single‐step cation‐exchange method for quantitative separation of trace levels of Li and Mg from multiple sample matrices. Methods The column method utilises the macro‐porous AGMP‐50 resin and a high‐aspect ratio column, allowing quantitative separation of Li and Mg from natural waters, sediments, rocks and carbonate matrices following the same elution protocol. High‐precision isotope determination was conducted by multi‐collector inductively coupled plasma mass spectrometry (MC‐ICPMS) on the Thermo Scientific™ NEPTUNE Plus™ fitted with 1013 Ω amplifiers which allow accurate and precise measurements at ion beams ≤0.51 V. Results Sub‐nanogram Li samples (0.3–0.5 ng) were regularly separated (yielding Mg masses of 1–70 μg) using the presented column method. The total sample consumption during isotopic analysis is <0.5 ng Li and <115 ng Mg with long‐term external 2σ precisions of ±0.39‰ for δ7Li and ±0.07‰ for δ26Mg. The results for geological reference standards and seawater analysed by our method are in excellent agreement with published values despite the order of magnitude lower sample consumption. Conclusions The possibility of eluting small sample masses and the low analytical sample consumption make this method ideal for samples of limited mass or low Li concentration, such as foraminifera, mineral separates or dilute river waters. PMID:29078008

Open tubular capillary columns with basic templates made by the generalized preparation protocol in capillary electrochromatography chiral separation and template structural effects on chiral separation capability.

PubMed

Zaidi, Shabi Abbas; Lee, Seung Mi; Cheong, Won Jo

2011-03-04

Some open tubular (OT) molecule imprinted polymer (MIP) silica capillary columns have been prepared using atenolol, sulpiride, methyl benzylamine (MBA) and (1-naphthyl)-ethylamine (NEA) as templates by the pre-established generalized preparation protocol. The four MIP thin layers of different templates showed quite different morphologies. The racemic selectivity of each MIP column for the template enantiomers was optimized by changing eluent composition and pH. The template structural effects on chiral separation performance have been examined. This work verifies the versatility of the generalized preparation protocol for OT-MIP silica capillary columns by extending its boundary toward templates with basic functional group moieties. This study is the very first report to demonstrate a generalized MIP preparation protocol that is valid for both acidic and basic templates. The chiral separation performances of atenolol and sulpiride by the MIPs of this study were found better than or comparable to those of atenolol and sulpiride obtained by non-MIP separation techniques and those of some basic template enantiomers obtained by MIP based techniques. Copyright © 2011 Elsevier B.V. All rights reserved.

Process and apparatus for separation of components of a gas stream

DOEpatents

Bryan, Charles R.; Torczynski, John R.; Brady, Patrick V.; Gallis, Michail; Brooks, Carlton F.

2014-06-17

A process and apparatus for separating a gas mixture comprising providing a slot in a gas separation channel (conceptualized as a laterally elongated Clusius-Dickel column), having a length through which a net cross-flow of the gas mixture may be established; applying a higher temperature to one side of the channel and a lower temperature on an opposite side of the channel thereby causing thermal-diffusion and buoyant-convection flow to occur in the slot; and establishing a net cross-flow of a gas mixture comprising at least one higher density gas component and at least one lower density gas component along the length of the slot, wherein the cross-flow causes, in combination with the convection flow, a spiraling flow in the slot; and wherein the spiral flow causes an increasing amount of separation of the higher density gas from the lower density gas along the length of the channel. The process may use one or more slots and/or channels.

Process and apparatus for separation of components of a gas stream

DOEpatents

Bryan, Charles R; Torczynski, John R; Brady, Patrick V; Gallis, Michail; Brooks, Carlton F

2013-09-17

A process and apparatus for separating a gas mixture comprising providing a slot in a gas separation channel (conceptualized as a laterally elongated Clusius-Dickel column), having a length through which a net cross-flow of the gas mixture may be established; applying a higher temperature to one side of the channel and a lower temperature on an opposite side of the channel thereby causing thermal-diffusion and buoyant-convection flow to occur in the slot; and establishing a net cross-flow of a gas mixture comprising at least one higher density gas component and at least one lower density gas component along the length of the slot, wherein the cross-flow causes, in combination with the convection flow, a spiraling flow in the slot; and wherein the spiral flow causes an increasing amount of separation of the higher density gas from the lower density gas along the length of the channel. The process may use one or more slots and/or channels.

Process and apparatus for separation of components of a gas stream

DOEpatents

Bryan, Charles R; Torczynski, John R; Brady, Patrick V; Gallis, Michail; Brooks, Carlton F

2013-11-19

A process and apparatus for separating a gas mixture comprising providing a slot in a gas separation channel (conceptualized as a laterally elongated Clusius-Dickel column), having a length through which a net cross-flow of the gas mixture may be established; applying a higher temperature to one side of the channel and a lower temperature on an opposite side of the channel thereby causing thermal-diffusion and buoyant-convection flow to occur in the slot; and establishing a net cross-flow of a gas mixture comprising at least one higher density gas component and at least one lower density gas component along the length of the slot, wherein the cross-flow causes, in combination with the convection flow, a spiraling flow in the slot; and wherein the spiral flow causes an increasing amount of separation of the higher density gas from the lower density gas along the length of the channel. The process may use one or more slots and/or channels.

[Separation and purification of the components in Trachelospermum jasminoides by two dimensional hydrophilic interaction liquid chromatography- reversed-phase liquid chromatography].

PubMed

Jia, Youmei; Cai, Jianfeng; Xin, Huaxia; Feng, Jiatao; Fu, Yanhui; Fu, Qing; Jin, Yu

2017-06-08

A preparative two dimensional hydrophilic interaction liquid chromatography/reversed-phase liquid chromatography (Pre-2D-HILIC/RPLC) method was established to separate and purify the components in Trachelospermum jasminoides . The pigments and strongly polar components were removed from the crude extract after the active carbon decolorization and solid phase extraction processes. A Click XIon column (250 mm×20 mm, 10 μm) was selected as stationary phase and water-acetonitrile as mobile phases in the first dimensional HILIC. Finally, 15 fractions were collected under UV-triggered mode. In the second dimensional RPLC, a C18 column (250 mm×20 mm, 5 μm) was selected and water-acetonitrile was used as mobile phases. As a result, 14 compounds with high purity were obtained, which were further identified by mass spectrometry (MS) and nuclear magnetic resonance (NMR). Finally, 11 lignan compounds and three flavonoid compounds were obtained. The method has a good orthogonality, and can improve the resolution and the peak capacity. It is significant for the separation of complex components from Trachelospermum jasminoides .

Separating Iso-Propanol-Toluene mixture by azeotropic distillation

NASA Astrophysics Data System (ADS)

Iqbal, Asma; Ahmad, Syed Akhlaq

2018-05-01

The separation of Iso-Propanol-Toluene azeotropic mixture using Acetone as an entrainer has been simulated on Aspen Plus software package using rigorous methods. Calculations of the vapor-liquid equilibrium for the binary system are done using UNIQUAC-RK model which gives a good agreement with the experimental data reported in literature. The effects of the Reflux ratio (RR), distillate-to-feed molar ratio (D/F), feed stage, solvent feed stage, Total no. of stages and solvent feed temperature on the product purities and recoveries are studied to obtain their optimum values that give the maximum purity and recovery of products. The configuration consists of 20 theoretical stages with an equimolar feed of binary mixture. The desired separation of binary mixture has been achieved at the feed stage and an entrainer feeding stage of 15 and 12 respectively with the reflux ratios of 2.5 and 4.0, and D/F ratio of 0.75 and 0.54 respectively in the two columns. The simulation results thus obtained are useful to setup the optimal column configuration of the azeotropic distillation process.

Classification of LC columns based on the QSRR method and selectivity toward moclobemide and its metabolites.

PubMed

Plenis, Alina; Olędzka, Ilona; Bączek, Tomasz

2013-05-05

This paper focuses on a comparative study of the column classification system based on the quantitative structure-retention relationships (QSRR method) and column performance in real biomedical analysis. The assay was carried out for the LC separation of moclobemide and its metabolites in human plasma, using a set of 24 stationary phases. The QSRR models established for the studied stationary phases were compared with the column test performance results under two chemometric techniques - the principal component analysis (PCA) and the hierarchical clustering analysis (HCA). The study confirmed that the stationary phase classes found closely related by the QSRR approach yielded comparable separation for moclobemide and its metabolites. Therefore, the QSRR method could be considered supportive in the selection of a suitable column for the biomedical analysis offering the selection of similar or dissimilar columns with a relatively higher certainty. Copyright © 2013 Elsevier B.V. All rights reserved.

SHINE and Mini-SHINE Column Designs for Recovery of Mo from 140 g-U/L Uranyl Sulfate

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

Stepinski, Dominique C.; Vandegrift, George F.

Argonne is assisting SHINE Medical Technologies (SHINE) in their efforts to develop an accelerator-driven process that utilizes a uranyl-sulfate solution for the production of fission Mo-99. In an effort to design a Mo-recovery system for the SHINE project using low-enriched uranium (LEU), we conducted batch, breakthrough, and pulse tests to determine the Mo isotherm, mass-transfer zone (MTZ), and system parameters for a 130 g-U/L uranyl sulfate solution at pH 1 and 80°C, as described previously. The VERSE program was utilized to calculate the MTZ under various loading times and velocities. The results were then used to design Mo separation andmore » recovery columns employing a pure titania sorbent (110-μm particles, S110, and 60 Å pore size). The plant-scale column designs assume Mo will be separated from 271 L of a 141 g-U/L uranyl sulfate solution, pH 1, containing 0.0023 mM Mo. The VERSE-designed recovery systems have been tested and verified in laboratory-scale experiments, and this approach was found to be very successful.« less

Nanoengineered analytical immobilized metal affinity chromatography stationary phase by atom transfer radical polymerization: Separation of synthetic prion peptides

PubMed Central

McCarthy, P.; Chattopadhyay, M.; Millhauser, G.L.; Tsarevsky, N.V.; Bombalski, L.; Matyjaszewski, K.; Shimmin, D.; Avdalovic, N.; Pohl, C.

2010-01-01

Atom transfer radical polymerization (ATRP) was employed to create isolated, metal-containing nanoparticles on the surface of non-porous polymeric beads with the goal of developing a new immobilized metal affnity chromatography (IMAC) stationary phase for separating prion peptides and proteins. Transmission electron microscopy was used to visualize nanoparticles on the substrate surface. Individual ferritin molecules were also visualized as ferritin–nanoparticle complexes. The column's resolving power was tested by synthesizing peptide analogs to the copper binding region of prion protein and injecting mixtures of these analogs onto the column. As expected, the column was capable of separating prion-related peptides differing in number of octapeptide repeat units (PHGGGWGQ), (PHGGGWGQ)2, and (PHGGGWGQ)4. Unexpectedly, the column could also resolve peptides containing the same number of repeats but differing only in the presence of a hydrophilic tail, Q → A substitution, or amide nitrogen methylation. PMID:17481564

Fingerprinting of traditional Chinese medicines on the C18-Diol mixed-mode column in online or offline two-dimensional liquid chromatography on the single column modes.

PubMed

Wang, Qing; Tong, Ling; Yao, Lin; Zhang, Peng; Xu, Li

2016-06-05

In the present study, a mixed-mode stationary phase, C18-Diol, was applied for fingerprint analysis of traditional Chinese medicines. Hydrophobic, hydrogen bonding and electrostatic interactions were demonstrated to contribute the retention separately or jointly, which endowed the C18-Diol stationary phase with distinct selectivity compared to the bare C18 one. The separation of total alkaloids extracted from Fritillaria hupehensis was compared on the C18-Diol and conventional C18 column with the greater resolving power and better symmetry responses on the former one. Besides, a novel two-dimensional liquid chromatography on the single column (2D-LC-1C) was realized on C18-Diol with the offline mode for the alcohol extract of Fritillaria hupehensis and online mode for Ligusticum chuanxiong Hort. The early co-eluted extracted components with great polarity on the first dimension were reinjected on the same column and well separated on the second dimension. The results exhibited that the two complementary RPLC and HILIC modes on C18-Diol stationary phase enhanced the separation capacity and revealed more abundant chemical information of the sample, which was a powerful tool in analyzing complex herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

The tropical precipitation pickup threshold and clouds in a radiative convective equilibrium model: 2. Two-layer moisture

NASA Astrophysics Data System (ADS)

Igel, Matthew R.

2017-06-01

This paper complements Part 1 in which cloud processes of aggregated convection are examined in a large-domain radiative convective equilibrium simulation in order to uncover those responsible for a consistently observed, abrupt increase in mean precipitation at a column relative humidity value of approximately 77%. In Part 2, the focus is on how the transition is affected independently by total moisture above and below the base of the melting layer. When mean precipitation rates are examined as simultaneous functions of these two moisture layers, four distinct behaviors are observed. These four behaviors suggest unique, yet familiar, physical regimes in which (i) little rain is produced by infrequent clouds, (ii) shallow convection produces increasing warm rain with increasing low-level moisture, (iii) deep convection produces progressively heavier rain above the transition point with increasing total moisture, and (iv) deep stratiform cloud produces increasingly intense precipitation from melting for increasing upper level moisture. The independent thresholds separating regimes in upper and lower layer humidity are shown to result in the value of total column humidity at which a transition between clear air and deep convection, and therefore a pickup in precipitation, is possible. All four regimes force atmospheric columns toward the pickup value at 77% column humidity, but each does so through a unique set of physical processes. Layer moisture and microphysical budgets are analyzed and contrasted with column budgets.

Multi-Column Xe/Kr Separation with AgZ-PAN and HZ-PAN

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

Greenhalgh, Mitchell Randy; Garn, Troy Gerry; Welty, Amy Keil

Previous multi-column xenon/krypton separation tests have demonstrated the capability of separating xenon from krypton in a mixed gas feed stream. The results of this initial testing with AgZ-PAN and HZ-PAN indicated that an excellent separation of xenon from krypton could be achieved. Building upon these initial results, a series of additional multi-column testing were performed in FY-16. The purpose of this testing was to scale up the sorbent beds, test a different composition of feed gas and attempt to improve the accuracy of the analysis of the individual capture columns’ compositions. Two Stirling coolers were installed in series to performmore » this testing. The use of the coolers instead of the cryostat provided two desired improvements, 1) removal of the large dilution due to the internal volume of the cryostat adsorption chamber, and 2) ability to increase the sorbent bed size for scale-up. The AgZ-PAN sorbent, due to its xenon selectivity, was loaded in the first column to capture the xenon while allowing the krypton to flow through and be routed to a second column containing the HZ-PAN for capture and analysis. The gases captured on both columns were sampled with evacuated sample bombs and subsequently analyzed via GC-MS for both krypton and xenon. The results of these tests can be used to develop the scope of future testing and analysis using this test bed for demonstrating the capture and separation of xenon and krypton using sorbents, for demonstrating desorption and regeneration of the sorbents, and for determining compositions of the desorbed gases. They indicate a need for future desorption studies in order to better quantify co-adsorbed species and final krypton purity.« less

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.

Separation of the Carotenoid Bixin from Annatto Seeds Using Thin-Layer and Column Chromatography

ERIC Educational Resources Information Center

McCullagh, James V.; Ramos, Nicholas

2008-01-01

In this experiment the carotenoid bixin is isolated from annatto ("Bixa orellana") seeds using column chromatography. The experiment has several key advantages over previous pigment separation experiments. First, unlike other experiments significant quantities of the carotenoid (typically 20 to 25 mg) can be isolated from small quantities of plant…

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.

Cavitating flow during water hammer using a generalized interface vaporous cavitation model

NASA Astrophysics Data System (ADS)

Sadafi, Mohamadhosein; Riasi, Alireza; Nourbakhsh, Seyed Ahmad

2012-10-01

In a transient flow simulation, column separation may occur when the calculated pressure head decreases to the saturated vapor pressure head in a computational grid. Abrupt valve closure or pump failure can result in a fast transient flow with column separation, potentially causing problems such as pipe failure, hydraulic equipment damage, cavitation or corrosion. This paper reports a numerical study of water hammer with column separation in a simple reservoir-pipeline-valve system and pumping station. The governing equations for two-phase transient flow in pipes are solved based on the method of characteristics (MOC) using a generalized interface vaporous cavitating model (GIVCM). The numerical results were compared with the experimental data for validation purposes, and the comparison indicated that the GIVCM describes the experimental results more accurately than the discrete vapor cavity model (DVCM). In particular, the GIVCM correlated better with the experimental data than the DVCM in terms of timing and pressure magnitude. The effects of geometric and hydraulic parameters on flow behavior in a pumping station with column separation were also investigated in this study.

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.

Separation of Ellagitannin-Rich Phenolics from U.S. Pecans and Chinese Hickory Nuts Using Fused-Core HPLC Columns and Their Characterization.

PubMed

Gong, Yi; Pegg, Ronald B

2017-07-19

U.S. pecans and Chinese hickory nuts possess a wide array of phenolic constituents with potential health benefits including phenolic acids and proanthocyanidins. Only limited information is available, however, on their compositions. The present study optimized the separation performance and characterized the low-molecular-weight phenolic fractions of these nuts with C18 and pentafluorophenyl (PFP) fused-core LC columns by employing a kinetic approach. Although both types of reversed-phase columns demonstrated similar performance in general, the PFP column furnished greater plate numbers and superior peak shapes for the low-molecular-weight fractions as well as overall separations of ellagic acid derivatives. The high-molecular-weight fraction of pecans, analyzed by a 3-μm HILIC column, possessed more proanthocyanidins than the Chinese hickory nuts with dimers and trimers (31.4 and 18.34 mg/g crude extract, respectively) being present at the greatest levels. Chinese hickory nuts had lower proanthocyanidin content but possessed tetramers and pentamers at 4.46 and 4.01 mg/g crude extract, respectively.

Radiochemical Applications of Insoluble Sulfate Columns. Analytical Possibilities in the Field of the Fission Product Solutions; APLICACIONES RADIO-QUIMICAS DE LAS COLUMNAS DE PRECIPITADOS DE SULFATOS INSOLUBLES. CONTRIBUCION AL ESTUDIO DE LAS SOLUCIONES ENVEJECIDAS DE PRODUCTOS DE FISION

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

Barrachina, M.; Sauvagnac, R.

1962-01-01

The heterogeneous ion-isotopic exchange column is used to determine the radiochemical composition of raw solutions used in the industrial recuperation of long-lived fission products, The separation of the radioelements is made by small columns, 1--3 cm height, of BaSO/sub 4/ or SrSO/sub 4/, under selected experimental conditions. These columns behave like inorganic exchangers, working by adsorption or ion-isotopic exchange depending on the cases, and they provide selective separation of fission products employing very small volumes of fixing and eluting solutions. By coupling the separative capabilities of these columns and the liquid--liquid extraction with the 2-thenoyltrifluoroacetone and the di-2 ethylexyl orthophosphoricmore » acid, a set of new radiochemical methods, for the determination of Sr/sup 90/, Y/sup 90/, Ce/sup 144/ - Pr/sup 144/, and Pm/sup 147/ in the fission product solutions of Marcoule, were developed. (auth)« less

Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

PubMed

Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

2011-01-01

We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

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.

Multi-Column Experimental Test Bed for Xe/Kr Separation

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

Greenhalgh, Mitchell Randy; Garn, Troy Gerry; Welty, Amy Keil

Previous research studies have shown that INL-developed engineered form sorbents are capable of capturing both Kr and Xe from various composite gas streams. The previous experimental test bed provided single column testing for capacity evaluations over a broad temperature range. To advance research capabilities, the employment of an additional column to study selective capture of target species to provide a defined final gas composition for waste storage was warranted. The second column addition also allows for compositional analyses of the final gas product to provide for final storage determinations. The INL krypton capture system was modified by adding an additionalmore » adsorption column in order to create a multi-column test bed. The purpose of this modification was to investigate the separation of xenon from krypton supplied as a mixed gas feed. The extra column was placed in a Stirling Ultra-low Temperature Cooler, capable of controlling temperatures between 190 and 253K. Additional piping and valves were incorporated into the system to allow for a variety of flow path configurations. The new column was filled with the AgZ-PAN sorbent which was utilized as the capture medium for xenon while allowing the krypton to pass through. The xenon-free gas stream was then routed to the cryostat filled with the HZ-PAN sorbent to capture the krypton at 191K. Selectivities of xenon over krypton were determined using the new column to verify the system performance and to establish the operating conditions required for multi-column testing. Results of these evaluations verified that the system was operating as designed and also demonstrated that AgZ-PAN exhibits excellent selectivity for xenon over krypton in air at or near room temperature. Two separation tests were performed utilizing a feed gas consisting of 1000 ppmv xenon and 150 ppmv krypton with the balance being made up of air. The AgZ-PAN temperature was held at 295 or 253K while the HZ-PAN was held at 191K for both tests. The effluent from the AgZ-PAN column was monitored via GC-TCD during the tests with no xenon being observed exiting the column during either test. Samples from each column were taken via evacuated sample bombs and were analyzed by GC-MS analysis. The results demonstrated the ability to separate xenon from krypton from a mixed gas feed utilizing the new multi-column system.« less

Highly crosslinked silicon polymers for gas chromatography columns

NASA Technical Reports Server (NTRS)

Shen, Thomas C. (Inventor)

1994-01-01

A new highly crosslinked silicone polymer particle for gas chromatography application and a process for synthesizing such copolymer are described. The new copolymer comprises vinyltriethoxysilane and octadecyltrichlorosilane. The copolymer has a high degree of crosslinking and a cool balance of polar to nonpolar sites in the porous silicon polymer assuring fast separation of compounds of variable polarity.

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.

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.

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.

Influence of sulfur-bearing polyatomic species on high precision measurements of Cu isotopic composition

USGS Publications Warehouse

Pribil, M.J.; Wanty, R.B.; Ridley, W.I.; Borrok, D.M.

2010-01-01

An increased interest in high precision Cu isotope ratio measurements using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) has developed recently for various natural geologic systems and environmental applications, these typically contain high concentrations of sulfur, particularly in the form of sulfate (SO42-) and sulfide (S). For example, Cu, Fe, and Zn concentrations in acid mine drainage (AMD) can range from 100??g/L to greater than 50mg/L with sulfur species concentrations reaching greater than 1000mg/L. Routine separation of Cu, Fe and Zn from AMD, Cu-sulfide minerals and other geological matrices usually incorporates single anion exchange resin column chromatography for metal separation. During chromatographic separation, variable breakthrough of SO42- during anion exchange resin column chromatography into the Cu fractions was observed as a function of the initial sulfur to Cu ratio, column properties, and the sample matrix. SO42- present in the Cu fraction can form a polyatomic 32S-14N-16O-1H species causing a direct mass interference with 63Cu and producing artificially light ??65Cu values. Here we report the extent of the mass interference caused by SO42- breakthrough when measuring ??65Cu on natural samples and NIST SRM 976 Cu isotope spiked with SO42- after both single anion column chromatography and double anion column chromatography. A set of five 100??g/L Cu SRM 976 samples spiked with 500mg/L SO42- resulted in an average ??65Cu of -3.50?????5.42??? following single anion column separation with variable SO42- breakthrough but an average concentration of 770??g/L. Following double anion column separation, the average SO42-concentration of 13??g/L resulted in better precision and accuracy for the measured ??65Cu value of 0.01?????0.02??? relative to the expected 0??? for SRM 976. We conclude that attention to SO42- breakthrough on sulfur-rich samples is necessary for accurate and precise measurements of ??65Cu and may require the use of a double ion exchange column procedure. ?? 2010.

Separation of scutellarin from crude extracts of Erigeron breviscapus (vant.) Hand. Mazz. by macroporous resins.

PubMed

Gao, Min; Huang, Wei; Liu, Chun-Zhao

2007-10-15

Scutellarin, a flavone glycoside, popularly used in the treatment of heart disease, has been efficiently separated using macroporous resins from crude extracts of Chinese medicinal plant Erigeron breviscapus (vant.) Hand. Mazz. HPD-800 resin offered the best adsorption and desorption capacity for scutellarin among the eight macroporous resins tested, and its adsorption data at 25 degrees C fit best to the Langmuir isotherm. The dynamic adsorption and desorption experiments have been carried out on a HPD-800 resin packed column to optimize the separation process of scutellarin from the crude extracts of E. breviscapus. After one run treatment with HPD-800 resin, the scutellarin content in the product was increased 15.69-fold from 2.61% to 40.96% with a recovery yield of 95.01%. The preparative separation process via adsorption-desorption method developed in this study provides a new approach for scale-up separation and purification of scutellarin for its wide pharmaceutical use.

Chromatographic column evaluation for the untargeted profiling of glucosinolates in cauliflower by means of ultra-high performance liquid chromatography coupled to high resolution mass spectrometry.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Montone, Carmela Maria; Piovesana, Susy; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2018-03-01

The untargeted profiling is a promising approach for the characterization of secondary metabolites in biological matrices. Thanks to the recent rapid development of high-resolution mass spectrometry (HRMS) instrumentations, the number of applications by untargeted approaches for biological samples profiling has widely increased in the recent years. Despite the high potentialities of HRMS, however, a major issue in natural products analysis often arises in the upstream process of compounds separation. A separation technique is necessary to avoid phenomena such as signal suppression, and it is especially needed in the presence of isomeric metabolites, which are otherwise indistinguishable. Glucosinolates (GLSs), a group of secondary metabolites widely distributed among plants, resulted to be associated to the prevention of some serious diseases, such as cancer. This led to the development of several methods for the analysis of GLSs in vegetables tissues. The issue of GLSs chromatographic separation has been widely studied in the past because of the difficulty in the analysis of this highly polar and variable class of compounds. Several alternatives to reversed phase (RP) chromatography, sometimes not compatible with the coupling of liquid chromatography with mass spectrometry, have been tested for the analysis of intact GLSs. However, the availability of new stationary phases, in the last years, could allow the re-evaluation of RP chromatography for the analysis of intact GLSs. In this work, a thorough evaluation of four RP chromatographic columns for the analysis of GLSs in cauliflower (Brassica oleracea L. var. botrytis) extracts by an ultra-high performance liquid chromatographic system coupled via electrospray source to a hybrid quadrupole-Orbitrap mass spectrometer is presented. The columns tested were the following: one column Luna Omega polar C 18 , one column Kinetex Biphenyl, one column Kinetex core-shell XB-C 18 , two columns Kinetex core-shell XB-C 18 . After a previous optimization of the extraction method, cauliflower extracts were analyzed testing four different mobile phases onto the four columns for a total of sixteen different chromatographic conditions. The chromatographic systems were evaluated based on the number of detected and tentatively identified GLSs. Luna Polar stationary phase resulted to be the most suitable for the analysis of GLSs compared to Kinetex XB and Kinetex Biphenyl columns stationary phase. However, two in series Kinetex XB columns increased the number of tentatively identified GLSs compared to one Kinetex XB, showing the importance of column length in the analysis of complex mixtures. The data obtained with the best chromatographic system were deeply analyzed by MS/MS investigation for the final identification. Fiflty-one GLSs were tentatively identified, 24 of which have never been identified in cauliflower. Finally the linearity of the analytes response over the analyzed range of concentration was checked, suggesting that the developed method is suitable for both qualitative and quantitative analysis of GLSs in phytochemical mixtures. Copyright © 2017 Elsevier B.V. All rights reserved.

Very high pressure liquid chromatography using core-shell particles: quantitative analysis of fast gradient separations without post-run times.

PubMed

Stankovich, Joseph J; Gritti, Fabrice; Stevenson, Paul G; Beaver, Lois A; Guiochon, Georges

2014-01-17

Five methods for controlling the mobile phase flow rate for gradient elution analyses using very high pressure liquid chromatography (VHPLC) were tested to determine thermal stability of the column during rapid gradient separations. To obtain rapid separations, instruments are operated at high flow rates and high inlet pressure leading to uneven thermal effects across columns and additional time needed to restore thermal equilibrium between successive analyses. The purpose of this study is to investigate means to minimize thermal instability and obtain reliable results by measuring the reproducibility of the results of six replicate gradient separations of a nine component RPLC standard mixture under various experimental conditions with no post-run times. Gradient separations under different conditions were performed: constant flow rates, two sets of constant pressure operation, programmed flow constant pressure operation, and conditions which theoretically should yield a constant net heat loss at the column's wall. The results show that using constant flow rates, programmed flow constant pressures, and constant heat loss at the column's wall all provide reproducible separations. However, performing separations using a high constant pressure with programmed flow reduces the analysis time by 16% compared to constant flow rate methods. For the constant flow rate, programmed flow constant pressure, and constant wall heat experiments no equilibration time (post-run time) was required to obtain highly reproducible data. Copyright © 2013 Elsevier B.V. All rights reserved.

Chelate-modified polymers for atmospheric gas chromatography

NASA Technical Reports Server (NTRS)

Christensen, W. W.; Mayer, L. A.; Woeller, F. H. (Inventor)

1980-01-01

Chromatographic materials were developed to serve as the stationary phase of columns used in the separation of atmospheric gases. These materials consist of a crosslinked porous polymer matrix, e.g., a divinylbenzene polymer, into which has been embedded an inorganic complexed ion such as N,N'-ethylene-bis-(acetylacetoniminato)-cobalt (2). Organic nitrogenous bases, such as pyridine, may be incorporated into the chelate polymer complexes to increase their chromatographic utility. With such materials, the process of gas chromatography is greatly simplified, especially in terms of time and quantity of material needed for a gas separation.

Chiral Separation of G-type Chemical Warfare Nerve Agents via Analytical Supercritical Fluid Chromatography

PubMed Central

Kasten, Shane A; Zulli, Steven; Jones, Jonathan L; Dephillipo, Thomas; Cerasoli, Douglas M

2014-01-01

Chemical warfare nerve agents (CWNAs) are extremely toxic organophosphorus compounds that contain a chiral phosphorus center. Undirected synthesis of G-type CWNAs produces stereoisomers of tabun, sarin, soman, and cyclosarin (GA, GB, GD, and GF, respectively). Analytical-scale methods were developed using a supercritical fluid chromatography (SFC) system in tandem with a mass spectrometer for the separation, quantitation, and isolation of individual stereoisomers of GA, GB, GD, and GF. Screening various chiral stationary phases (CSPs) for the capacity to provide full baseline separation of the CWNAs revealed that a Regis WhelkO1 (SS) column was capable of separating the enantiomers of GA, GB, and GF, with elution of the P(+) enantiomer preceding elution of the corresponding P(–) enantiomer; two WhelkO1 (SS) columns had to be connected in series to achieve complete baseline resolution. The four diastereomers of GD were also resolved using two tandem WhelkO1 (SS) columns, with complete baseline separation of the two P(+) epimers. A single WhelkO1 (RR) column with inverse stereochemistry resulted in baseline separation of the GD P(–) epimers. The analytical methods described can be scaled to allow isolation of individual stereoisomers to assist in screening and development of countermeasures to organophosphorus nerve agents. Chirality 26:817–824, 2014. © 2014 The Authors. Chirality published by John Wiley Periodicals, Inc. PMID:25298066

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.

A novel design of reactive distillation configuration for 2-methoxy-2-methylheptane process

NASA Astrophysics Data System (ADS)

Hussain, Arif; Qyyum, Muhammad Abdul; Quang Minh, Le; Jimin, Hong; Lee, Moonyong

2017-11-01

The study aims to reveal the possibility of reactive distillation (RD) in the 2-methoxy-2-methylheptane (MMH) production process. MMH is getting more industrial and academic interests as a gasoline additive to replace methyl tert-butyl ether. Traditionally, MMH is obtained by carrying out the reaction in the reactor followed by three distillation columns. The high yield of MMH could be achieved by keeping the large reactor size or by using the large excess of 2-methyl-1-heptene (MH). Both former and latter strategies are associated with the high capital and operating costs. To solve these problems, this study proposed an innovative RD configuration to take synergistic benefits of reaction and separation involved. This innovative RD configuration allows the production of MMH with significantly lower capital, operating and total annual costs. For desired MMH yield, the result demonstrates that the proposed RD configuration can reduce energy, capital, and total annual costs up to 7.7, 31.3, and 17.1%, respectively, compared to a conventional process. Furthermore, the influence of some important design parameters on the RD column performance was also explored to overcome the temperature limitation of acid resin catalyst inside the reactive zone of the RD column.

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.

Gradient stationary phase optimized selectivity liquid chromatography with conventional columns.

PubMed

Chen, Kai; Lynen, Frédéric; Szucs, Roman; Hanna-Brown, Melissa; Sandra, Pat

2013-05-21

Stationary phase optimized selectivity liquid chromatography (SOSLC) is a promising technique to optimize the selectivity of a given separation. By combination of different stationary phases, SOSLC offers excellent possibilities for method development under both isocratic and gradient conditions. The so far available commercial SOSLC protocol utilizes dedicated column cartridges and corresponding cartridge holders to build up the combined column of different stationary phases. The present work is aimed at developing and extending the gradient SOSLC approach towards coupling conventional columns. Generic tubing was used to connect short commercially available LC columns. Fast and base-line separation of a mixture of 12 compounds containing phenones, benzoic acids and hydroxybenzoates under both isocratic and linear gradient conditions was selected to demonstrate the potential of SOSLC. The influence of the connecting tubing on the deviation of predictions is also discussed.

Column Testing and 1D Reactive Transport Modeling to Evaluate Uranium Plume Persistence Processes

NASA Astrophysics Data System (ADS)

Johnson, R. H.; Morrison, S.; Morris, S.; Tigar, A.; Dam, W. L.; Dayvault, J.

2015-12-01

At many U.S. Department of Energy Office of Legacy Management sites, 100 year natural flushing was selected as a remedial option for groundwater uranium plumes. However, current data indicate that natural flushing is not occurring as quickly as expected and solid-phase and aqueous uranium concentrations are persistent. At the Grand Junction, Colorado office site, column testing was completed on core collected below an area where uranium mill tailings have been removed. The total uranium concentration in this core was 13.2 mg/kg and the column was flushed with laboratory-created water with no uranium and chemistry similar to the nearby Gunnison River. The core was flushed for a total of 91 pore volumes producing a maximum effluent uranium concentration of 6,110 μg/L at 2.1 pore volumes and a minimum uranium concentration of 36.2 μg/L at the final pore volume. These results indicate complex geochemical reactions at small pore volumes and a long tailing affect at greater pore volumes. Stop flow data indicate the occurrence of non-equilibrium processes that create uranium concentration rebound. These data confirm the potential for plume persistence, which is occurring at the field scale. 1D reactive transport modeling was completed using PHREEQC (geochemical model) and calibrated to the column test data manually and using PEST (inverse modeling calibration routine). Processes of sorption, dual porosity with diffusion, mineral dissolution, dispersion, and cation exchange were evaluated separately and in combination. The calibration results indicate that sorption and dual porosity are major processes in explaining the column test data. These processes are also supported by fission track photographs that show solid-phase uranium residing in less mobile pore spaces. These procedures provide valuable information on plume persistence and secondary source processes that may be used to better inform and evaluate remedial strategies, including natural flushing.

Layer-by-layer self-assembled graphene oxide/silica microsphere composites as stationary phase for high performance liquid chromatography.

PubMed

Liang, Xiaojing; Liu, Shujuan; Song, Xinwang; Zhu, Yangwen; Jiang, Shengxiang

2012-11-21

Graphene oxide (GO) has been layer-by-layer assembled onto silica microspheres to form a GO/SiO(2) composite stationary phase. All the characterizations of GO/SiO(2) by elemental analysis, Raman spectroscopy and Fourier transformed infrared spectrometry confirmed that with the increase of the assembled layer, GO gradually increases on the silica surface. The chromatographic properties of bare SiO(2) and GO/SiO(2) with different GO assembled layers show that the amount of GO plays an important role in the separation of analytes. Only the appropriate amount of GO on SiO(2) can perform a good chromatographic separation. The comparison between chromatographic performances of bare SiO(2) column, GO/SiO(2)-2 column and C18 commercial column clearly show that GO/SiO(2)-2 and C18 columns obtained a better separation; GO/SiO(2)-2 exhibits a large π-electron system and C18 exhibits hydrophobicity. The eluting order, peak width and resolution of analyte on GO/SiO(2)-2 column was highly dependent on the size of its π-electron system, while on the C18 column the decisive factor is its hydrophobic property.

Group type analysis of asphalt by column liquid chromatography

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

Zhang, C.; Yang, J.; Xue, Y.

2008-07-01

An improved analysis method for characterization of asphalt was established. The method is based on column chromatography technique. The asphalts were separated into four groups: saturates, aromatics, resins, and asphaltenes, quantitatively. About 0.1 g of sample was required in each analysis. About 20 mL of n-heptanes was used to separate out saturates first. Then about 35 mL of n-heptanes/dichloromethane (.5, v/v) mixture was used to separate out aromatics. About 30 mL of dichloromethane/tetrahydrofuran (1/3, v/v) mixture was used to separate out resin. The quality of the separation was confirmed by infrared spectra (IR) and {sup 1}H NMR analysis. The modelmore » compounds, tetracosan for saturates, dibenz(o)anthracen for aromatics, and acetanilide for resins were used for verification. The IR and {sup 1}H NMR analysis of the prepared fractions from the column liquid chromatography were in good agreement that of pure reagents.« less

DETERMINATION OF PESTICIDES IN COMPOSITE DIETARY SAMPLES BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY IN THE SELECTED ION MONITORING MODE USING A TEMPERATURE PROGRAMMABLE LARGE VOLUME INJECTOR WITH PRE-SEPARATION COLUMN

EPA Science Inventory

Use of a temperature-programmable pre-separation column in the gas chromatographic injection port permits determination of a wide range of semi-volatile pesticides including organochlorines, organophosphates, triazines, and anilines in fatty composite dietary samples while reduci...

HPLC separation post-column reaction, UV-visible and fluorescence detection of trace UO/sub 2//sup 2 +//U/sup 4 +/ species in aqueous solutions

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

Karimi, A.R.

In this study a method for the measurement of uranium in natural waters at sub-ppB concentration levels by the separation and determination of U/sup 4 +/ and UO/sub 2//sup 2 +/ species is proposed. Reversed phase high performance liquid chromatography, followed by a post-column reaction and a sensitive UV-visible detection system was the method of choice to determine qualitatively and quantitatively the two uranium species. Also a cation-exchange and fluorescence detection system was studied for separation and determination of UO/sub 2//sup 2 +/ ions. Uranyl ion was selectively complexed with L-phenylalanine moetie in the sample solution containing U/sup 4 +/more » ions. Uranium (IV)/U(VI)-ligand was separated on a C/sub 18/ column with acetate buffer. Hexanesulfonate was found to be the choice for ion-pair reagent. The separation was best done with the acetate buffer at .01 M concentration and pH of 3.5. Absorption of the two species were measured after a post-column reaction with Arsenazo-III. Chromatographic parameters were calculated and a calibration curves were constructed. The detection limit for the procedure was 0.7 ..mu..g/mo and 1.2..mu..g/ml for U(IV) and U(VI) respectively. When U(VI) was separated on the cation-exchange column the limit of detection was calculated to be 1 ..mu..g/ml. The direct fluorometric method for U(VI) measurement results in a detection limit of 2 ppB and upper concentration limit of 2 ppM. The effect of interfering ions in the direct method of determination could be eliminated by dilution of sample solution.« less

Evaluating the energy performance of a hybrid membrane-solvent process for flue gas carbon dioxide capture

DOE PAGES

Kusuma, Victor A.; Li, Zhiwei; Hopkinson, David; ...

2016-10-13

In this study, a particularly energy intensive step in the conventional amine absorption process to remove carbon dioxide is solvent regeneration using a steam stripping column. An attractive alternative to reduce the energy requirement is gas pressurized stripping, in which a high pressure noncondensable gas is used to strip CO 2 off the rich solvent stream. The gas pressurized stripping column product, having CO 2 at high concentration and high partial pressure, can then be regenerated readily using membrane separation. In this study, we performed an energetic analysis in the form of total equivalent work and found that, for capturingmore » CO 2 from flue gas, this hybrid stripping process consumes 49% less energy compared to the base case conventional MEA absorption/steam stripping process. We also found the amount of membrane required in this process is much less than required for direct CO 2 capture from the flue gas: approximately 100-fold less than a previously published two-stage cross-flow scheme, mostly due to the more favorable pressure ratio and CO 2 concentration. There does exist a trade-off between energy consumption and required membrane area that is most strongly affected by the gas pressurized stripper operating pressure. While initial analysis looks promising from both an energy requirement and membrane unit capital cost, the viability of this hybrid process depends on the availability of advanced, next generation gas separation membranes to perform the stripping gas regeneration.« less

Evaluating the energy performance of a hybrid membrane-solvent process for flue gas carbon dioxide capture

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

Kusuma, Victor A.; Li, Zhiwei; Hopkinson, David

In this study, a particularly energy intensive step in the conventional amine absorption process to remove carbon dioxide is solvent regeneration using a steam stripping column. An attractive alternative to reduce the energy requirement is gas pressurized stripping, in which a high pressure noncondensable gas is used to strip CO 2 off the rich solvent stream. The gas pressurized stripping column product, having CO 2 at high concentration and high partial pressure, can then be regenerated readily using membrane separation. In this study, we performed an energetic analysis in the form of total equivalent work and found that, for capturingmore » CO 2 from flue gas, this hybrid stripping process consumes 49% less energy compared to the base case conventional MEA absorption/steam stripping process. We also found the amount of membrane required in this process is much less than required for direct CO 2 capture from the flue gas: approximately 100-fold less than a previously published two-stage cross-flow scheme, mostly due to the more favorable pressure ratio and CO 2 concentration. There does exist a trade-off between energy consumption and required membrane area that is most strongly affected by the gas pressurized stripper operating pressure. While initial analysis looks promising from both an energy requirement and membrane unit capital cost, the viability of this hybrid process depends on the availability of advanced, next generation gas separation membranes to perform the stripping gas regeneration.« less

Hydrodynamic chromatography of macromolecules using polymer monolithic columns.

PubMed

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

2011-12-02

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

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

Egorov, Oleg; O'Hara, Matthew J.; Grate, Jay W.

An automated fluidic instrument is described that rapidly determines the total 99Tc content of aged nuclear waste samples, where the matrix is chemically and radiologically complex and the existing speciation of the 99Tc is variable. The monitor links microwave-assisted sample preparation with an automated anion exchange column separation and detection using a flow-through solid scintillator detector. The sample preparation steps acidify the sample, decompose organics, and convert all Tc species to the pertechnetate anion. The column-based anion exchange procedure separates the pertechnetate from the complex sample matrix, so that radiometric detection can provide accurate measurement of 99Tc. We developed amore » preprogrammed spike addition procedure to automatically determine matrix-matched calibration. The overall measurement efficiency that is determined simultaneously provides a self-diagnostic parameter for the radiochemical separation and overall instrument function. Continuous, automated operation was demonstrated over the course of 54 h, which resulted in the analysis of 215 samples plus 54 hly spike-addition samples, with consistent overall measurement efficiency for the operation of the monitor. A sample can be processed and measured automatically in just 12.5 min with a detection limit of 23.5 Bq/mL of 99Tc in low activity waste (0.495 mL sample volume), with better than 10% RSD precision at concentrations above the quantification limit. This rapid automated analysis method was developed to support nuclear waste processing operations planned for the Hanford nuclear site.« less

Characterization and applications of reversed-phase column selectivity based on the hydrophobic-subtraction model.

PubMed

Marchand, D H; Snyder, L R; Dolan, J W

2008-05-16

A total of 371 reversed-phase columns have now been characterized in terms of selectivity, based on five solute-column interactions (the hydrophobic-subtraction model). The present study illustrates the use of these data for interpreting peak-tailing and column stability. New insights are also provided concerning column selectivity as a function of ligand and silica type, and the selection of columns for orthogonal separations is re-examined. Some suggestions for the quality control of reversed-phase columns during manufacture are offered.

Simple, rapid, and environmentally friendly method for the separation of isoflavones using ultra-high performance supercritical fluid chromatography.

PubMed

Wu, Wenjie; Zhang, Yuan; Wu, Hanqiu; Zhou, Weie; Cheng, Yan; Li, Hongna; Zhang, Chuanbin; Li, Lulu; Huang, Ying; Zhang, Feng

2017-07-01

Isoflavones are natural substances that exhibit hormone-like pharmacological activities. The separation of isoflavones remains an analytical challenge because of their similar structures. We show that ultra-high performance supercritical fluid chromatography can be an appropriate tool to achieve the fast separation of 12 common dietary isoflavones. Among the five tested columns the Torus DEA column was found to be the most effective column for the separation of these isoflavones. The impact of individual parameters on the retention time and separation factor was evaluated. These parameters were optimized to develop a simple, rapid, and green method for the separation of the 12 target analytes. It only took 12.91 min using gradient elution with methanol as an organic modifier and formic acid as an additive. These isoflavones were determined with limit of quantitation ranging from 0.10 to 0.50 μg/mL, which was sufficient for reliable determination of various matrixes. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Centrifugal precipitation chromatography

PubMed Central

Ito, Yoichiro; Lin, Qi

2009-01-01

Centrifugal precipitation chromatography separates analytes according their solubility in ammonium sulfate (AS) solution and other precipitants. The separation column is made from a pair of long spiral channels partitioned with a semipermeable membrane. In a typical separation, concentrated ammonium sulfate is eluted through one channel while water is eluted through the other channel in the opposite direction. The countercurrent process forms an exponential AS concentration gradient through the water channel. Consequently, protein samples injected into the water channel is subjected to a steadily increasing AS concentration and at the critical AS concentration they are precipitated and deposited in the channel bed by the centrifugal force. Then the chromatographic separation is started by gradually reducing the AS concentration in the AS channel which lowers the AS gradient concentration in the water channel. This results in dissolution of deposited proteins which are again precipitated at an advanced critical point as they move through the channel. Consequently, proteins repeat precipitation and dissolution through a long channel and finally eluted out from the column in the order of their solubility in the AS solution. The present method has been successfully applied to a number of analytes including human serum proteins, recombinant ketosteroid isomerase, carotenoid cleavage enzymes, plasmid DNA, polysaccharide, polymerized pigments, PEG-protein conjugates, etc. The method is capable to single out the target species of proteins by affinity ligand or immunoaffinity separation. PMID:19541553

Temperature-enhanced alumina HPLC method for the analysis of wax esters, sterol esters, and methyl esters.

PubMed

Moreau, Robert A; Kohout, Karen; Singh, Vijay

2002-12-01

Previous attempts at separating nonpolar lipid esters (including wax esters, sterol esters, and methyl esters) have achieved only limited success. Among the several normal-phase methods tested, a single recent report of a method employing an alumina column at 30 degrees C with a binary gradient system was the most promising. In the current study, modification of the alumina method by increasing the column temperature to 75 degrees C improved the separation of standards of wax esters and sterol esters. Elevated column temperature also enhanced the separation of FAME with differing degrees of unsaturation. Evidence was also presented to indicate that the method similarly separated phytosterol esters, based on their levels of unsaturation. With the increased interest in phytosterol- and phytostanol-ester enriched functional foods, this method should provide a technique to characterize and compare these products.

New analytical spiral tube assembly for separation of proteins by counter-current chromatography.

PubMed

Ma, Xiaofeng; Ito, Yoichiro

2015-07-31

A new spiral column assembly for analytical separation by counter-current chromatography is described. The column is made from a plastic spiral tube support which has 12 interwoven spiral grooves. The PTFE tubing of 1.6mm ID was first flattened by extruding through a narrow slit and inserted into the grooves to make 5 spiral layers with about 60ml capacity. The performance of the spiral column assembly was tested with separation of three stable protein samples including cytochrome C, myoglobin and lysozyme in a polymer phase system composed of polyethylene glycol 1000 and dibasic potassium phosphate each at 12.5% (w/w) in water. At 2ml/min, three protein samples were well resolved in 1h. The separation time may be further shortened by application of higher revolution speed and flow rate by improving the strength of the spiral tube support in the future. Published by Elsevier B.V.

Comparison of analytical protein separation characteristics for three amine-based capillary-channeled polymer (C-CP) stationary phases.

PubMed

Jiang, Liuwei; Marcus, R Kenneth

2016-02-01

Capillary-channeled polymer (C-CP) fiber stationary phases are finding utility in the realms of protein analytics as well as downstream processing. We have recently described the modification of poly(ethylene terephthalate) (PET) C-CP fibers to affect amine-rich phases for the weak anion-exchange (WAX) separation of proteins. Polyethylenimine (PEI) is covalently coupled to the PET surface, with subsequent cross-linking imparted by treatment with 1,4-butanediol diglycidyl ether (BUDGE). These modifications yield vastly improved dynamic binding capacities over the unmodified fibers. We have also previously employed native (unmodified) nylon 6 C-CP fibers as weak anion/cation-exchange (mixed-mode) and hydrophobic interaction chromatography (HIC) phases for protein separations. Polyamide, nylon 6, consists of amide groups along the polymer backbone, with primary amines and carboxylic acid end groups. The analytical separation characteristics of these three amine-based C-CP fiber phases are compared here. Each of the C-CP fiber columns in this study was shown to be able to separate a bovine serum albumin/hemoglobin/lysozyme mixture at high mobile phase linear velocity (∼70 mm s(-1)) but with different elution characteristics. These differences reflect the types of protein-surface interactions that are occurring, based on the active group composition of the fiber surfaces. This study provides important fundamental understanding for the development of surface-modified C-CP fiber columns for protein separation.

Theoretical study of closed-loop recycling liquid-liquid chromatography and experimental verification of the theory.

PubMed

Kostanyan, Artak E; Erastov, Andrey A

2016-09-02

The non-ideal recycling equilibrium-cell model including the effects of extra-column dispersion is used to simulate and analyze closed-loop recycling counter-current chromatography (CLR CCC). Previously, the operating scheme with the detector located before the column was considered. In this study, analysis of the process is carried out for a more realistic and practical scheme with the detector located immediately after the column. Peak equation for individual cycles and equations describing the transport of single peaks and complex chromatograms inside the recycling closed-loop, as well as equations for the resolution between single solute peaks of the neighboring cycles, for the resolution of peaks in the recycling chromatogram and for the resolution between the chromatograms of the neighboring cycles are presented. It is shown that, unlike conventional chromatography, increasing of the extra-column volume (the recycling line length) may allow a better separation of the components in CLR chromatography. For the experimental verification of the theory, aspirin, caffeine, coumarin and the solvent system hexane/ethyl acetate/ethanol/water (1:1:1:1) were used. Comparison of experimental and simulated processes of recycling and distribution of the solutes in the closed-loop demonstrated a good agreement between theory and experiment. Copyright © 2016 Elsevier B.V. All rights reserved.

Mineral Separation in a CELSS by Ion-exchange Chromatography

NASA Technical Reports Server (NTRS)

Ballou, E. V.; Spitze, L. A.; Wong, F. W.; Wydeven, T.; Johnson, C. C.

1982-01-01

Operational parameters pertinent to ion exchange chromatography separation were identified. The experiments were performed with 9 mm diameter ion exchange columns and conventional column accessories. The cation separation beds were packed with AG 50W-X2 strong acid cation exchange resin in H(+) form and 200-400 dry mesh particle size. The stripper beds used in some experiments were packed with AG 1-XB strong base cation exchange resin in OH(-) form and 200-400 dry mesh particle size.

METHOD FOR REMOVAL OF LIGHT ISOTOPE PRODUCT FROM LIQUID THERMAL DIFFUSION UNITS

DOEpatents

Hoffman, J.D.; Ballou, J.K.

1957-11-19

A method and apparatus are described for removing the lighter isotope of a gaseous-liquid product from a number of diffusion columns of a liquid thermal diffusion system in two stages by the use of freeze valves. The subject liquid flows from the diffusion columns into a heated sloping capsule where the liquid is vaporized by the action of steam in a heated jacket surrounding the capsule. When the capsule is filled the gas flows into a collector. Flow between the various stages is controlled by freeze valves which are opened and closed by the passage of gas and cool water respectively through coils surrounding portions of the pipes through which the process liquid is passed. The use of the dual stage remover-collector and the freeze valves is an improvement on the thermal diffusion separation process whereby the fraction containing the lighter isotope many be removed from the tops of the diffusion columns without intercolumn flow, or prior stage flow while the contents of the capsule is removed to the final receiver.

Method and apparatus for the selective separation of gaseous coal gasification products by pressure swing adsorption

DOEpatents

Ghate, Madhav R.; Yang, Ralph T.

1987-01-01

Bulk separation of the gaseous components of multi-component gases provided by the gasification of coal including hydrogen, carbon monoxide, methane, and acid gases (carbon dioxide plus hydrogen sulfide) are selectively adsorbed by a pressure swing adsorption technique using activated carbon, zeolite or a combination thereof as the adsorbent. By charging a column containing the adsorbent with a gas mixture and pressurizing the column to a pressure sufficient to cause the adsorption of the gases and then reducing the partial pressure of the contents of the column, the gases are selectively and sequentially desorbed. Hydrogen, the least absorbable gas of the gaseous mixture, is the first gas to be desorbed and is removed from the column in a co-current direction followed by the carbon monoxide, hydrogen and methane. With the pressure in the column reduced to about atmospheric pressure the column is evacuated in a countercurrent direction to remove the acid gases from the column. The present invention is particularly advantageous as a producer of high parity hydrogen from gaseous products of coal gasification and as an acid gas scrubber.

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.

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.

Capillary electrochromatography of inorganic cations in open tubular columns with a controllable capacity multilayered stationary phase architecture.

PubMed

Kubán, Pavel; Kubán, Petr; Kubán, Vlastimil; Hauser, Peter C; Bocek, Petr

2008-05-09

In this paper capillary electrochromatography of alkali and alkaline-earth metal cations in open tubular capillary columns is described. Capillary columns are prepared by coating fused silica capillaries of 75 microm I.D. with poly(butadiene-maleic acid) copolymer (PBMA) in multiple layers. Thermally initiated radical polymerization is used to crosslink the stationary phase. Capillary columns with different number of stationary phase layers can be prepared and allow for the adjustment of separation selectivity in the electrochromatographic mode. Fast and sensitive separations of common inorganic cations are achieved in less than 6 min in a 60 cm capillary column with on-column capacitively coupled contactless conductivity detector. Limits of detection (S/N=3) for the determination of alkali and alkaline-earth metal cations range from 0.3 to 2.5 microM and repeatability is better than 0.5, 4.5 and 6.1% for migration times, peak heights and peak areas, respectively.

Induced natural convection thermal cycling device

DOEpatents

Heung, Leung Kit [Aiken, SC

2002-08-13

A device for separating gases, especially isotopes, by thermal cycling of a separation column using a pressure vessel mounted vertically and having baffled sources for cold and heat. Coils at the top are cooled with a fluid such as liquid nitrogen. Coils at the bottom are either electrical resistance coils or a tubular heat exchange. The sources are shrouded with an insulated "top hat" and simultaneously opened and closed at the outlets to cool or heat the separation column. Alternatively, the sources for cold and heat are mounted separately outside the vessel and an external loop is provided for each circuit.

First high-resolution stratigraphic column of the Martian north polar layered deposits

USGS Publications Warehouse

Fishbaugh, K.E.; Hvidberg, C.S.; Byrne, S.; Russell, P.S.; Herkenhoff, K. E.; Winstrup, M.; Kirk, R.

2010-01-01

This study achieves the first high-spatial-resolution, layer-scale, measured stratigraphic column of the Martian north polar layered deposits using a 1m-posting DEM. The marker beds found throughout the upper North Polar Layered Deposits range in thickness from 1.6 m-16.0 m +/-1.4 m, and 6 of 13 marker beds are separated by ???25-35 m. Thin-layer sets have average layer separations of 1.6 m. These layer separations may account for the spectral-power-peaks found in previous brightness-profile analyses. Marker-bed layer thicknesses show a weak trend of decreasing thickness with depth that we interpret to potentially be the result of a decreased accumulation rate in the past, for those layers. However, the stratigraphic column reveals that a simple rhythmic or bundled layer sequence is not immediately apparent throughout the column, implying that the relationship between polar layer formation and cyclic climate forcing is quite complex. Copyright ?? 2010 by the American Geophysical Union.

First high-resolution stratigraphic column of the Martian north polar layered deposits

NASA Astrophysics Data System (ADS)

Fishbaugh, Kathryn E.; Hvidberg, Christine S.; Byrne, Shane; Russell, Patrick S.; Herkenhoff, Kenneth E.; Winstrup, Mai; Kirk, Randolph

2010-04-01

This study achieves the first high-spatial-resolution, layer-scale, measured stratigraphic column of the Martian north polar layered deposits using a 1m-posting DEM. The marker beds found throughout the upper North Polar Layered Deposits range in thickness from 1.6 m-16.0 m +/- 1.4 m, and 6 of 13 marker beds are separated by ˜25-35 m. Thin-layer sets have average layer separations of 1.6 m. These layer separations may account for the spectral-power-peaks found in previous brightness-profile analyses. Marker-bed layer thicknesses show a weak trend of decreasing thickness with depth that we interpret to potentially be the result of a decreased accumulation rate in the past, for those layers. However, the stratigraphic column reveals that a simple rhythmic or bundled layer sequence is not immediately apparent throughout the column, implying that the relationship between polar layer formation and cyclic climate forcing is quite complex.

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.

Particle detector spatial resolution

DOEpatents

Perez-Mendez, V.

1992-12-15

Method and apparatus for producing separated columns of scintillation layer material, for use in detection of X-rays and high energy charged particles with improved spatial resolution is disclosed. A pattern of ridges or projections is formed on one surface of a substrate layer or in a thin polyimide layer, and the scintillation layer is grown at controlled temperature and growth rate on the ridge-containing material. The scintillation material preferentially forms cylinders or columns, separated by gaps conforming to the pattern of ridges, and these columns direct most of the light produced in the scintillation layer along individual columns for subsequent detection in a photodiode layer. The gaps may be filled with a light-absorbing material to further enhance the spatial resolution of the particle detector. 12 figs.

Cu2+-imprinted cross-linked chitosan resin as micro-column packing materials for online chemiluminescence determination of trace copper.

PubMed

Nie, Feng; Hao, Liang; Gao, Mei; Wu, Yingchun; Li, Xinsheng; Yu, Sha

2011-01-01

The Cu(2+)-imprinted cross-linked chitosan resin was synthesized and the binding characteristic of the resin to Cu(2+) was evaluated. The prepared resin was packed into a micro-glass column and used as micro-separating column. The micro-separating column was connected into the chemiluminescence flow system and placed in front of the window of the photomultiplier tube. Based on the luminol-hydrogen peroxide chemiluminescence system, a flow injection online chemiluminescence method for determination of trace copper was developed and trace Cu(2+) in complex samples was successfully determined. The proposed method improved the shortcomings of chemiluminescence method's poor selectivity. Copyright © 2010 John Wiley & Sons, Ltd.

Particle detector spatial resolution

DOEpatents

Perez-Mendez, Victor

1992-01-01

Method and apparatus for producing separated columns of scintillation layer material, for use in detection of X-rays and high energy charged particles with improved spatial resolution. A pattern of ridges or projections is formed on one surface of a substrate layer or in a thin polyimide layer, and the scintillation layer is grown at controlled temperature and growth rate on the ridge-containing material. The scintillation material preferentially forms cylinders or columns, separated by gaps conforming to the pattern of ridges, and these columns direct most of the light produced in the scintillation layer along individual columns for subsequent detection in a photodiode layer. The gaps may be filled with a light-absorbing material to further enhance the spatial resolution of the particle detector.

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.

Experiments on water detritiation and cryogenic distillation at TLK; Impact on ITER fuel cycle subsystems interfaces

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

Cristescu, I.; Cristescu, I. R.; Doerr, L.

2008-07-15

The ITER Isotope Separation System (ISS) and Water Detritiation System (WDS) should be integrated in order to reduce potential chronic tritium emissions from the ISS. This is achieved by routing the top (protium) product from the ISS to a feed point near the bottom end of the WDS Liquid Phase Catalytic Exchange (LPCE) column. This provides an additional barrier against ISS emissions and should mitigate the memory effects due to process parameter fluctuations in the ISS. To support the research activities needed to characterize the performances of various components for WDS and ISS processes under various working conditions and configurationsmore » as needed for ITER design, an experimental facility called TRENTA representative of the ITER WDS and ISS protium separation column, has been commissioned and is in operation at TLK The experimental program on TRENTA facility is conducted to provide the necessary design data related to the relevant ITER operating modes. The operation availability and performances of ISS-WDS have impact on ITER fuel cycle subsystems with consequences on the design integration. The preliminary experimental data on TRENTA facility are presented. (authors)« less

Measurement of actinides and strontium-90 in high activity waste

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

Maxwell, S.L. III; Nelson, M.R.

1994-08-01

The reliable measurement of trace radionuclides in high activity waste is important to support waste processing activities at SRS (F and H Area Waste Tanks, Extended Sludge Processing (ESP) and In-Tank precipitation (ITP) processing). Separation techniques are needed to remove high levels of gamma activity and alpha/beta interferences prior to analytical measurement. Using new extraction chromatographic resins from EiChrom Industries, Inc., the SRS Central Laboratory has developed new high speed separation methods that enable measurement of neptunium, thorium, uranium, plutonium, americium and strontium-90 in high activity waste solutions. Small particle size resin and applied vacuum are used to reduce analysismore » times and enhance column performance. Extraction chromatographic resins are easy to use and eliminate the generation of contaminated liquid organic waste.« less

Continuous recovery of valine in a model mixture of amino acids and salt from Corynebacterium bacteria fermentation using a simulated moving bed chromatography.

PubMed

Park, Chanhun; Nam, Hee-Geun; Jo, Se-Hee; Wang, Nien-Hwa Linda; Mun, Sungyong

2016-02-26

The economical efficiency of valine production in related industries is largely affected by the performance of a valine separation process, in which valine is to be separated from leucine, alanine, and ammonium sulfate. Such separation is currently handled by a batch-mode hybrid process based on ion-exchange and crystallization schemes. To make a substantial improvement in the economical efficiency of an industrial valine production, such a batch-mode process based on two different separation schemes needs to be converted into a continuous-mode separation process based on a single separation scheme. To address this issue, a simulated moving bed (SMB) technology was applied in this study to the development of a continuous-mode valine-separation chromatographic process with uniformity in adsorbent and liquid phases. It was first found that a Chromalite-PCG600C resin could be eligible for the adsorbent of such process, particularly in an industrial scale. The intrinsic parameters of each component on the Chromalite-PCG600C adsorbent were determined and then utilized in selecting a proper set of configurations for SMB units, columns, and ports, under which the SMB operating parameters were optimized with a genetic algorithm. Finally, the optimized SMB based on the selected configurations was tested experimentally, which confirmed its effectiveness in continuous separation of valine from leucine, alanine, ammonium sulfate with high purity, high yield, high throughput, and high valine product concentration. It is thus expected that the developed SMB process in this study will be able to serve as one of the trustworthy ways of improving the economical efficiency of an industrial valine production process. Copyright © 2016 Elsevier B.V. All rights reserved.

Trace analysis of impurities in bulk gases by gas chromatography-pulsed discharge helium ionization detection with "heart-cutting" technique.

PubMed

Weijun, Yao

2007-10-12

A method has been developed for the detection of low-nL/L-level impurities in bulk gases such as H(2), O(2), Ar, N(2), He, methane, ethylene and propylene, respectively. The solution presented here is based upon gas chromatography-pulsed discharge helium ionization detection (GC-PDHID) coupled with three two-position valves, one two-way solenoid valve and four packed columns. During the operation, the moisture and heavy compounds are first back-flushed via a pre-column. Then the trace impurities (except CO(2) which is diverted to a separate analytical column for separation and detection) together with the matrix enter onto a main column, followed by the heart-cut of the impurities onto a longer analytical column for complete separation. Finally the detection is performed by PDHID. This method has been applied to different bulk gases and the applicability of detecting impurities in H(2), Ar, and N(2) are herewith demonstrated. As an example, the resulting detection limit of 100 nL/L and a dynamic range of 100-1000 nL/L have been obtained using an Ar sample containing methane.

Preparation and characterization of lysine-immobilized poly(glycidyl methacrylate) nanoparticle-coated capillary for the separation of amino acids by open tubular capillary electrochromatography.

PubMed

Xu, Liang; Cui, Pengfei; Wang, Dongmei; Tang, Cheng; Dong, Linyi; Zhang, Can; Duan, Hongquan; Yang, Victor C

2014-01-03

In this study, poly(glycidyl methacrylate) (PGMA) nanoparticles (NPs) were prepared and chemically immobilized for the first time onto a capillary inner wall for open tubular capillary electrochromatography (OTCEC). The immobilization of PGMA NPs onto the capillary was attained by a ring-opening reaction between the NPs and an amino-silylated fused capillary inner surface. Scanning electron micrographs clearly demonstrated that the NPs were bound to the capillary inner surface in a dense monolayer. The PGMA NP-coated column was then functionalized by lysine (Lys). After fuctionalization, the capillary can afford strong anodic electroosmotic flow, especially in acidic running buffers. Separations of three amino acids (including tryptophan, tyrosine and phenylalanine) were performed in NP-modified, monolayer Lys-functionalized and bare uncoated capillaries. Results indicated that the NP-coated column can provide more retention and higher resolution for analytes due to the hydrophobic interaction between analytes and the NP-coating. Run-to-run and column-to-column reproducibilities in the separation of the amino acids using the NP-modified column were also demonstrated. Copyright © 2013 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.

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

PubMed

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

2017-11-01

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

Growth of second stage mineral in Lytechinus variegatus.

PubMed

Stock, S R; Seto, Jong; Deymier, A C; Rack, A; Veis, A

2017-10-30

Purpose and Aims: Sea urchin teeth consist of calcite and form in two stages with different magnesium contents. The first stage structures of independently formed plates and needle-prisms define the shape of the tooth, and the columns of the second stage mineral cements the first stage structures together and control the fracture behavior of the mature tooth. This study investigates the nucleation and growth of the second stage mineral. Scanning electron microscopy (SEM) and synchrotron microComputed Tomography characterized the structures of the second phase material found in developing of Lytechinus variegatus teeth. Although the column development is a continuous process, defining four phases of column formation captures the changes that occur in teeth of L. variegatus. The earliest phase consists of small 1-2 µm diameter hemispheres, and the second of 5-10 µm diameter, mound-like structures with a nodular surface, develops from the hemispheres. The mounds eventually bridge the syncytium between adjacent plates and form hyperboloid structures (phase three) that appear like mesas when plates separate during the fracture. The mesa diameter increases with time until the column diameter is significantly larger than its height, defining the fourth phase of column development. Energy dispersive x-ray spectroscopy confirms that the columns contain more magnesium than the underlying plates; the ratios of magnesium to calcium are consistent with compositions derived from x-ray diffraction. Columns grow from both bounding plates. The presence of first phase columns interspersed among third stage mesas indicates very localized control of mineralization.

Pretreatment method for immunoassay of polychlorinated biphenyls in transformer oil using multilayer capillary column and microfluidic liquid-liquid partitioning.

PubMed

Aota, Arata; Date, Yasumoto; Terakado, Shingo; Ohmura, Naoya

2013-01-01

Polychlorinated biphenyls (PCBs) are persistent organic pollutants that are present in the insulating oil inside a large number of transformers. To aid in eliminating PCB-contaminated transformers, PCBs in oil need to be measured using a rapid and cost-effective analytical method. We previously reported a pretreatment method for the immunoassay of PCBs in oil using a large-scale multilayer column and a microchip with multiple microrecesses, which permitted concentrated solvent extraction. In this paper, we report on a more rapid and facile pretreatment method, without an evaporation process, by improving the column and the microchip. In a miniaturized column, the decomposition and separation of oil were completed in 2 min. PCBs can be eluted from the capillary column at concentrations seven-times higher than those from the previous column. The total volume of the microrecesses was increased by improving the microrecess structure, the enabling extraction of four-times the amount of PCBs achieved with the previous system. By interfacing the capillary column with the improved microchip, PCBs in the eluate from the column were extracted into dimethyl sulfoxide in microrecesses with high enrichment and without the need for evaporation. Pretreatment was completed within 20 min. The pretreated oil was analyzed using a flow-based kinetic exclusion immunoassay. The limit of detection of PCBs in oil was 0.15 mg kg(-1), which satisfies the criterion set in Japan of 0.5 mg kg(-1).

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

PubMed

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

2018-05-15

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

Enrichment and separation of chlorogenic acid from the extract of Eupatorium adenophorum Spreng by macroporous resin.

PubMed

Liu, Boyan; Dong, Beitao; Yuan, Xiaofan; Kuang, Qirong; Zhao, Qingsheng; Yang, Mei; Liu, Jie; Zhao, Bing

2016-01-01

A simple and efficient chromatographic method for separation of chlorogenic acid from Eupatorium adenophorum Spreng extract was developed. The adsorption properties of nine macroporous resins were evaluated. NKA-II resin showed much better adsorption/desorption properties. The adsorption of chlorogenic acid on NKA-II resin at 25°C was well fitted to Langmuir isotherm model and pseudo-second-order kinetic model. The dynamic adsorption and desorption experiments were carried out on columns packed with NKA-II resin to optimize the separation process. The content of chlorogenic acid in the product increased to 22.17%, with a recovery yield of 82.41%. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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

2008-06-01

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

Simultaneous determination of diastereoisomeric and enantiomeric impurities in SSS-octahydroindole-2-carboxylic acid by chiral high-performance liquid chromatography with pre-column derivatization.

PubMed

Wang, Jin Zhao; Zeng, Su; Hu, Gong Yun; Wang, Dan Hua

2009-04-10

SSS-Octahydroindole-2-carboxylic acid (SSS-Oic) is a key intermediate used in the synthesis of some angiotensin-converting enzyme (ACE) inhibitors. The separation of diastereoisomers and enantiomers of Oic was performed using a pre-column derivatization chiral HPLC method. Phenyl isothiocyanate (PITC) was used as the derivatization reagent. Three PITC derivatives of Oic stereoisomers were separated on an Ultron ES-OVM chiral column (150 mm x 4.6 mm, 5 microm). Derivatization conditions such as reaction temperature, reaction time and derivatization reagent concentration were investigated. The chromatographic conditions for separation of the three PITC-Oic derivatives were optimized. The method was successfully applied in the diastereoisomeric and enantiomeric purity test of SSS-Oic.

Preparative electrophoresis of living lymphocytes

NASA Technical Reports Server (NTRS)

Vanoss, C. J.; Bigazzi, P. E.; Gillman, C. F.; Allen, R. E.

1974-01-01

Vertical liquid columns containing low molecular weight dextran density gradients can be used for preparative lymphocyte electrophoresis on earth, in simulation of 0 gravity conditions. Another method that has been tested at 1 G, is the electrophoresis of lymphocytes in a upward direction in vertical columns. By both methods up to 10 to the 7th power lymphocytes can be separated at one time in a 30 cm glass column of 8 mm inside diameter, at 12 v/cm, in 2 hours. Due to convection and sedimentation problems, the separation at 1 G is less than ideal, but it is expected that at 0 gravity electrophoresis will prove to be a uniquely powerful cell separation tool. The technical feasibility of electrophoresing inert particles at 0 G has been proven earlier, during the flight of Apollo 16.

SEPARATION OF THORIUM FROM URANIUM

DOEpatents

Bane, R.W.

1959-09-01

A description is given for the separation of thorium from uranium by forming an aqueous acidic solution containing ionic species of thorium, uranyl uranium, and hydroxylamine, flowing the solution through a column containing the phenol-formaldehyde type cation exchange resin to selectively adsorb substantially all the thorium values and a portion of the uranium values, flowing a dilute solution of hydrochloric acid through the column to desorb the uranium values, and then flowing a dilute aqueous acidic solution containing an ion, such as bisulfate, which has a complexing effect upon thortum through the column to desorb substantially all of the thorium.

FRACTIONATING COLUMN PRODUCT COLLECTOR CONTROL

DOEpatents

Paxson, G.D. Jr.

1964-03-10

Means for detecting minute fluid products from a chemical separation column and for advancing a collector tube rack in order to automatically separate and collect successive fractionated products are described. A charge is imposed on the forming drops at the column orifice to create an electric field as the drop falls in the vicinity of a sensing plate. The field is detected by an electrometer tube coupled to the plate causing an output signal to actuate rotation of a collector turntable rack, thereby positioning new collectors under the orifice. The invention provides reliable automatic collection independent of drop size, rate of fall, or chemical composition. (AEC)

Application of a chromatography model with linear gradient elution experimental data to the rapid scale-up in ion-exchange process chromatography of proteins.

PubMed

Ishihara, Takashi; Kadoya, Toshihiko; Yamamoto, Shuichi

2007-08-24

We applied the model described in our previous paper to the rapid scale-up in the ion exchange chromatography of proteins, in which linear flow velocity, column length and gradient slope were changed. We carried out linear gradient elution experiments, and obtained data for the peak salt concentration and peak width. From these data, the plate height (HETP) was calculated as a function of the mobile phase velocity and iso-resolution curve (the separation time and elution volume relationship for the same resolution) was calculated. The scale-up chromatography conditions were determined by the iso-resolution curve. The scale-up of the linear gradient elution from 5 to 100mL and 2.5L column sizes was performed both by the separation of beta-lactoglobulin A and beta-lactoglobulin B with anion-exchange chromatography and by the purification of a recombinant protein with cation-exchange chromatography. Resolution, recovery and purity were examined in order to verify the proposed method.

Development of a nucleotide sugar purification method using a mixed mode column & mass spectrometry detection.

PubMed

Eastwood, Heather; Xia, Fang; Lo, Mei-Chu; Zhou, Jing; Jordan, John B; McCarter, John; Barnhart, Wesley W; Gahm, Kyung-Hyun

2015-11-10

Analysis of nucleotide sugars, nucleoside di- and triphosphates and sugar-phosphates is an essential step in the process of understanding enzymatic pathways. A facile and rapid separation method was developed to analyze these compounds present in an enzymatic reaction mixture utilized to produce nucleotide sugars. The Primesep SB column explored in this study utilizes hydrophobic interactions as well as electrostatic interactions with the phosphoric portion of the nucleotide sugars. Ammonium formate buffer was selected due to its compatibility with mass spectrometry. Negative ion mode mass spectrometry was adopted for detection of the sugar phosphate (fucose-1-phophate), as the compound is not amenable to UV detection. Various mobile phase conditions such as pH, buffer concentration and organic modifier were explored. The semi-preparative separation method was developed to prepare 30mg of the nucleotide sugar. (19)F NMR was utilized to determine purity of the purified fluorinated nucleotide sugar. The collected nucleotide sugar was found to be 99% pure. Published by Elsevier B.V.

Fast, high peak capacity separations in comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry.

PubMed

Fitz, Brian D; Wilson, Ryan B; Parsons, Brendon A; Hoggard, Jamin C; Synovec, Robert E

2012-11-30

Peak capacity production is substantially improved for two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS) and applied to the fast separation of a 28 component liquid test mixture, and two complex vapor samples (a 65 component volatile organic compound test mixture, and the headspace of warm ground coffee beans). A high peak capacity is achieved in a short separation time by selecting appropriate experimental conditions based on theoretical modeling of on-column band broadening, and by reducing the off-column band broadening by applying a narrow, concentrated injection pulse onto the primary column using high-speed cryo-focusing injection (HSCFI), referred to as thermal injection. A long, relatively narrow open tubular capillary column (20 m, 100 μm inner diameter (i.d.) with a 0.4 μm film thickness to benefit column capacity) was used as the primary column. The initial flow rate was 2 ml/min (60 cm/s average linear flow velocity) which is slightly below the optimal average linear gas velocity of 83 cm/s, due to the flow rate constraint of the TOFMS vacuum system. The oven temperature programming rate was 30°C/min. The secondary column (1.8m, 100 μm i.d. with a 0.1 μm film thickness) provided a relatively high peak capacity separation, concurrent with a significantly shorter modulation period, P(M), than commonly applied with the commercial instrument. With this GC×GC-TOFMS instrumental platform, compounds in the 28 component liquid test mixture provided a ∼7 min separation (with a ∼6.5 min separation time window), producing average peak widths of ∼600 ms full width half maximum (FWHM), resulting in a peak capacity on the primary column of ∼400 peaks (at unit resolution). Using a secondary column with a 500 ms P(M), average peak widths of ∼20 ms FWHM were achieved, thus providing a peak capacity of 15 peaks on the second dimension. Overall, an ideal orthogonal GC×GC peak capacity of ∼6000 peaks (at unit resolution) was achieved (or a β-corrected orthogonal peak capacity of ∼4400, at an average modulation ratio, M(R), of ∼2). This corresponds to an ideal orthogonal peak capacity production of ∼1000 peaks/min (or ∼700 peaks/min, β-corrected). For comparison, standard split/split-less injection techniques with a 1:100 split, when combined with standard GC×GC conditions typically provide a peak capacity production of ∼100 peaks/min, hence the instrumental platform we report provides a ∼7-fold to 10-fold improvement. Copyright © 2012 Elsevier B.V. All rights reserved.

Evaluation and application of a mixed-mode chromatographic stationary phase in two-dimensional liquid chromatography for the separation of traditional Chinese medicine.

PubMed

Wei, Zhishen; Fu, Qing; Cai, Jianfeng; Huan, Liyun; Zhao, Jianchao; Shi, Hui; Jin, Yu; Liang, Xinmiao

2016-06-01

In this study, two mixed-mode chromatography stationary phases (C8SAX and C8SCX) were evaluated and used to establish a two-dimensional liquid chromatography system for the separation of traditional Chinese medicine. The chromatographic properties of the mixed-mode columns were systematically evaluated by comparing with other three columns of C8, strong anion exchanger, and strong cation exchanger. The result showed that C8SAX and C8SCX had a mixed-mode retention mechanism including electrostatic interaction and hydrophobic interaction. Especially, they were suitable for separating acidic and/or basic compounds and their separation selectivities could be easily adjusted by changing pH value. Then, several off-line 2D-LC systems based on the C8SAX in the first dimension and C8SAX, C8SCX, or C8 columns in the second dimension were developed to analyze a traditional Chinese medicine-Uncaria rhynchophylla. The two-dimensional liquid chromatography system of C8SAX (pH 3.0) × C8SAX (pH 6.0) exhibited the most effective peak distribution. Finally, fractions of U. rhynchophylla prepared from the first dimension were successfully separated on the C8SAX column with a gradient pH. Thus, the mixed-mode stationary phase could provide a platform to separate the traditional Chinese medicine in practical applications. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Method of component assay of alpha-glucosyltransferase-treated stevia (enzymatically modified stevia) products using enzymatic hydrolysis].

PubMed

Hirata, Keiko; Shimamura, Yasuhiro; Suzuki, Keiko; Sadamasu, Yuki; Ito, Koichi

2005-12-01

We have developed an analytical method for components of alpha-glucosyltransferase-treated stevia, a food additive product. Suitable conditions to separate additional sugar from alpha-glucosyltransferase-treated stevia by using glucoamylase were found (55 degrees C for 3 hr with 250 U of glucoamylase in 10 mL of reaction solution). By solid-phase extraction using a C18 cartridge column, polysaccharides were excluded from the sample, and the glycosides and sugar obtained after hydrolysis with glucoamylase were separated on another C18 cartridge column. The glycosides and sugar contents were determined by HPLC. By this method, additional sugar was detected in all of three product samples tested and the sugar was glucose. The contents of glucose and total glycosides (minus unreacted glycoside) were 25-42% and 35.7-52.5%, respectively. In alpha-glucosyltransferase-treated stevia, the sum of total glycosides and glucose amounted to 77.5-80.4% of the total and their recoveries from samples from which polysaccharide had been excluded by C18 cartridge column processing were over 85%. The contents of alpha-glucosyltransferase-treated stevia obtained by multiplying the sugar content by the coefficient (0.9) for hydrolysis and converting on dry weight basis were all over 80.0% and met the standard set by the Japan Food Additives Association.

Mitigating an increase of specific power consumption in a cryogenic air separation unit at reduced oxygen production

NASA Astrophysics Data System (ADS)

Singla, Rohit; Chowdhury, Kanchan

2017-02-01

Specific power consumed in a Linde double column air separation unit (ASU) increases as the quantity of oxygen produced at a given purity is decreased due to the changes of system requirement or market demand. As the plant operates in part load condition, the specific power consumption (SPC) increases as the total power consumption remains the same. In order to mitigate the increase of SPC at lower oxygen production, the operating pressure of high pressure column (HPC) can be lowered by extending the low pressure column (LPC) by a few trays and adding a second reboiler. As the duty of second reboiler in LPC is increased, the recovery of oxygen decreases with a lowering of the HPC pressure. This results in mitigation of the increase of SPC of the plant. A Medium pressure ASU with dual reboiler that produces pressurised gaseous and liquid products of oxygen and nitrogen is simulated in Aspen Hysys 8.6®, a commercial process simulator to determine SPC at varying oxygen production. The effects of reduced pressure of air feed into the cold box on the size of heat exchangers (HX) are analysed. Operation strategy to obtain various oxygen production rates at varying demand is also proposed.

Optimization of microfabricated nanoliter-scale solid-phase extraction device for detection of gel-separated proteins in low abundance by matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Chen, Wenzhang; Shen, Jing; Yin, Xuefeng; Yu, Yingnian

2007-01-01

A nano-scale solid-phase extraction (SPE) device was developed for the detection of gel-separated proteins in low abundance by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) with a simplified microfabrication technology. By using SU-8 photoresist instead of epoxy glue to connect the microchannel and transfer capillary, polymeric contaminant signals in MS analysis were significantly reduced. Micro SPE columns with different capacities and geometric characteristics were investigated in order to increase the detection sensitivity and decrease spot size for MALDI-TOF-MS analysis. It is shown that enhancements in sensitivities for the detection of proteins in low abundance were correlated with the reduction in column capacity and increase in column aspect ratio. Fifty nanoliters of matrix solution were sufficient to elute the sample completely from the optimized micro SPE column with 3.5 nL capacity. The mass spectrum of a 5 fmol in-gel tryptic digest of bovine serum albumin (BSA), processed by the micro SPE column, demonstrated that 29 peptides matched the protein giving a sequence coverage of 51%, which was better than that obtained from analysis of 25 fmol of the same sample prepared by the dried-droplet method. With the micro SPE column treatment of 2 microL of digestion supernatant of a gel spot of the IQGAP1 protein, 15 peptides were detected from the mass spectrum with the highest individual score of 111, while, with a ZipTip procedure, only nine peaks were detected with the highest individual score of 71. Analytical results demonstrated that this approach greatly improved the sequence coverage and identification specificity for the tested protein. It can serve as a very useful tool in proteomics studies, especially for low abundance proteins. Copyright (c) 2006 John Wiley & Sons, Ltd.

Process for the separation and purification of yttrium-90 for medical applications

DOEpatents

Horwitz, P.E.; Dietz, M.L.

1994-11-29

An extraction chromatographic method for the preparation of [sup 90]Y of high chemical and radiochemical purity is disclosed. After an initial purification of a [sup 90]Sr stock solution and a suitable period of [sup 90]Y ingrowth, the solution is passed through a series of strontium-selective chromatographic columns, each of which lowers the [sup 90]Sr content of the mixture by a factor of about 10[sup 3]. The [sup 90]Y remaining is freed from any residual [sup 90]Sr, from its [sup 90]Zr daughter, and from any remaining impurities by passing the sample through a final column designed to selectively retain yttrium. 5 figures.

Short-cut Methods versus Rigorous Methods for Performance-evaluation of Distillation Configurations

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

Ramapriya, Gautham Madenoor; Selvarajah, Ajiththaa; Jimenez Cucaita, Luis Eduardo

Here, this study demonstrates the efficacy of a short-cut method such as the Global Minimization Algorithm (GMA), that uses assumptions of ideal mixtures, constant molar overflow (CMO) and pinched columns, in pruning the search-space of distillation column configurations for zeotropic multicomponent separation, to provide a small subset of attractive configurations with low minimum heat duties. The short-cut method, due to its simplifying assumptions, is computationally efficient, yet reliable in identifying the small subset of useful configurations for further detailed process evaluation. This two-tier approach allows expedient search of the configuration space containing hundreds to thousands of candidate configurations for amore » given application.« less

Short-cut Methods versus Rigorous Methods for Performance-evaluation of Distillation Configurations

DOE PAGES

Ramapriya, Gautham Madenoor; Selvarajah, Ajiththaa; Jimenez Cucaita, Luis Eduardo; ...

2018-05-17

Here, this study demonstrates the efficacy of a short-cut method such as the Global Minimization Algorithm (GMA), that uses assumptions of ideal mixtures, constant molar overflow (CMO) and pinched columns, in pruning the search-space of distillation column configurations for zeotropic multicomponent separation, to provide a small subset of attractive configurations with low minimum heat duties. The short-cut method, due to its simplifying assumptions, is computationally efficient, yet reliable in identifying the small subset of useful configurations for further detailed process evaluation. This two-tier approach allows expedient search of the configuration space containing hundreds to thousands of candidate configurations for amore » given application.« less

A process for the separation and purification of yttrium-90 for medical applications

DOEpatents

Horwitz, P.E.; Dietz, M.L.

1993-01-01

An extraction chromatographic method for the preparation of {sup 90}Y of high chemical and radiochemical purity is disclosed. After an initial purification of a {sup 90}Sr stock solution and a suitable period of {sup 90}Y ingrowth, the solution is passed through a series of strontium-selective chromatographic columns, each of which lowers the {sup 90}Sr content of the mixture by a factor of about 10{sup 3}. The {sup 90}Y remaining is freed from any residual {sup 90}Sr, from its {sup 90}Zr daughter, and from any remaining impurities by passing the sample through a final column designed to selectively retain yttrium.

Process for the separation and purification of yttrium-90 for medical applications

DOEpatents

Horwitz, Philip E.; Dietz, Mark L.

1994-01-01

An extraction chromatographic method for the preparation of .sup.90 Y of high chemical and radiochemical purity is disclosed. After an initial purification of a .sup.90 Sr stock solution and a suitable period of .sup.90 Y ingrowth, the solution is passed through a series of strontium-selective chromatographic columns, each of which lowers the .sup.90 Sr content of the mixture by a factor of about 10.sup.3. The .sup.90 Y remaining is freed from any residual .sup.90 Sr, from its .sup.90 Zr daughter, and from any remaining impurities by passing the sample through a final column designed to selectively retain yttrium.

Design of a Fission 99 Mo Recovery Process and Implications toward Mo Adsorption Mechanism on Titania and Alumina Sorbents

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

Stepinski, Dominique C.; Youker, Amanda J.; Krahn, Elizabeth O.

2017-03-01

Molybdenum-99 is a parent of the most widely used medical isotope technetium-99m. Proliferation concerns have prompted development of alternative Mo production methods utilizing low enriched uranium. Alumina and titania sorbents were evaluated for separation of Mo from concentrated uranyl nitrate solutions. System, mass transfer, and isotherm parameters were determined to enable design of Mo separation processes under a wide range of conditions. A model-based approach was utilized to design representative commercial-scale column processes. The designs and parameters were verified with bench-scale experiments. The results are essential for design of Mo separation processes from irradiated uranium solutions, selection of support materialmore » and process optimization. Mo uptake studies show that adsorption decreases with increasing concentration of uranyl nitrate; howeveL, examination of Mo adsorption as a function of nitrate ion concentration shows no dependency, indicating that uranium competes with Mo for adsorption sites. These results are consistent with reports indicating that Mo forms inner-sphere complexes with titania and alumina surface groups.« less

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

NASA Astrophysics Data System (ADS)

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

2017-03-01

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

Isoelectric focusing of red blood cells in a density gradient stabilized column

NASA Technical Reports Server (NTRS)

Smolka, A. J. K.; Miller, T. Y.

1980-01-01

The effects of Ficoll and cell application pH on red blood cell electrophoretic mobility and focusing pH were investigated by focusing cells in a density gradient stabilized column. Sample loading, cell dispersion, column conductivity, resolution of separation, and the effect of Ampholines were examined.

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

PubMed

Lísa, Miroslav; Holcapek, Michal; Sovová, Helena

2009-11-20

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

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.

Performance comparison of three types of high-speed counter-current chromatographs for the separation of components of hydrophilic and hydrophobic color additives.

PubMed

Weisz, Adrian; Ito, Yoichiro

2011-09-09

The performance of three types of high-speed counter-current chromatography (HSCCC) instruments was assessed for their use in separating components in hydrophilic and hydrophobic dye mixtures. The HSCCC instruments compared were: (i) a J-type coil planet centrifuge (CPC) system with a conventional multilayer-coil column, (ii) a J-type CPC system with a spiral-tube assembly-coil column, and (iii) a cross-axis CPC system with a multilayer-coil column. The hydrophilic dye mixture consisted of a sample of FD&C Blue No. 2 that contained mainly two isomeric components, 5,5'- and 5,7'-disulfonated indigo, in the ratio of ∼7:1. The hydrophobic dye mixture consisted of a sample of D&C Red No. 17 (mainly Sudan III) and Sudan II in the ratio of ∼4:1. The two-phase solvent systems used for these separations were 1-butanol/1.3M HCl and hexane/acetonitrile. Each of the three instruments was used in two experiments for the hydrophilic dye mixture and two for the hydrophobic dye mixture, for a total of 12 experiments. In one set of experiments, the lower phase was used as the mobile phase, and in the second set of experiments, the upper phase was used as the mobile phase. The results suggest that: (a) use of a J-type instrument with either a multilayer-coil column or a spiral-tube assembly column, applying the lower phase as the mobile phase, is preferable for separating the hydrophilic components of FD&C Blue No. 2; and (b) use of a J-type instrument with multilayer-coil column, while applying either the upper phase or the lower phase as the mobile phase, is preferable for separating the hydrophobic dye mixture of D&C Red No. 17 and Sudan II. Published by Elsevier B.V.

Separation of granulocytes from whole blood by leukoadhesion, phase 1

NASA Technical Reports Server (NTRS)

1976-01-01

Capillary glass tubes are investigated for the separation and retrieval of large quantities of viable granulocytes and monocytes from whole blood on a continuous basis from a single donor. This effort represented the feasibility demonstration of a three phase program for development of a capillary tube cell separation device. The activity included the analysis and parametric laboratory testing with subscale models required to design a prototype device. Capillary tubes 40 cm long with a nominal 0.030 cm internal diameter yielded the highest total process efficiency. Recovery efficiencies as high as 89% of the adhering cell population were obtained. Granulocyte phagocytosis of latex particles indicated approximately 90% viability. Monocytes recovered from the separation column retained their capability to stimulate human bone marrow colony growth, as demonstrated in an in vitro cell culture assay.

Two multidimensional chromatographic methods for enantiomeric analysis of o,p'-DDT and o,p'-DDD in contaminated soil and air in a malaria area of South Africa.

PubMed

Naudé, Yvette; Rohwer, Egmont R

2012-06-12

In rural parts of South Africa the organochlorine insecticide DDT (1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane) is still used for malaria vector control where traditional dwellings are sprayed on the inside with small quantities of technical DDT. Since o,p'-DDT may show enantioselective oestrogenicity and biodegradability, it is important to analyse enantiomers of o,p'-DDT and its chiral degradation product, o,p'-DDD, for both health and environmental-forensic considerations. Generally, chiral analysis is performed using heart-cut multidimensional gas chromatography (MDGC) and, more recently, comprehensive two-dimensional gas chromatography (GC×GC). We developed an off-line gas chromatographic fraction collection (heart-cut) procedure for the selective capturing of the appropriate isomers from a first apolar column, followed by reinjection and separation on a second chiral column. Only the o,p'-isomers of DDT and DDD fractions from the first dimension complex chromatogram (achiral apolar GC column separation) were selectively collected onto a polydimethylsiloxane (PDMS) multichannel open tubular silicone rubber trap by simply placing the latter device on the flame tip of an inactivated flame ionisation detector (FID). The multichannel trap containing the o,p'-heart-cuts was then thermally desorbed into a GC with time-of-flight mass spectrometry detection (GC-TOFMS) for second dimension enantioselective separation on a chiral column (β-cyclodextrin-based). By selectively capturing only the o,p'-isomers from the complex sample chromatogram, (1)D separation of ultra-trace level enantiomers could be achieved on the second chiral column without matrix interference. Here, we present solventless concentration techniques for extraction of DDT from contaminated soil and air, and report enantiomeric fraction (EF) values of o,p'-DDT and o,p'-DDD obtained by a new multidimensional approach for heart-cut gas chromatographic fraction collection for off-line second dimension enantiomeric separation by (1)D GC-TOFMS of selected isomers. This multidimensional method is compared to the complementary technique of comprehensive GC×GC-TOFMS using the same enantioselective column, this time as the first dimension of separation. Copyright © 2012 Elsevier B.V. All rights reserved.

The development of the super-biodiesel production continuously from Sunan pecan oil through the process of reactive distillation

NASA Astrophysics Data System (ADS)

Yohana, Eflita; Yulianto, Moh. Endy; Ikhsan, Diyono; Nanta, Aditya Marga; Puspitasari, Ristiyanti

2016-06-01

In general, a vegetable oil-based biodiesel production commercially operates a batch process with high investments and operational costs. Thus, it is necessary to develop super-biodiesel production from sunan pecan oil continuously through the process of reactive distillation. There are four advantages of the reactive distillation process for the biodiesel production, as follows: (i) it incorporates the process of transesterification reaction, and product separation of residual reactants become one stage of the process, so it saves the investment and operation costs, (ii) it reduces the need for raw materials because the methanol needed corresponds to the stoichiometry, so it also reduces the operation costs, (iii) the holdup time in the column is relatively short (5±0,5 minutes) compared to the batch process (1-2 hours), so it will reduce the operational production costs, and (iv) it is able to shift the reaction equilibrium, because the products and reactants that do not react are instantly separated (based on Le Chatelier's principles) so the conversion will be increased. However, the very crucial problem is determining the design tools and process conditions in order to maximize the conversion of the transesterification reaction in both phases. Thus, the purpose of this research was to design a continuous reactive distillation process by using a recycled condensate to increase the productivity of the super-biodiesel from sunan pecan oil. The research was carried out in three stages including (i) designing and fabricating the reactive distillation equipment, (ii) testing the tool performance and the optimization of the biodiesel production, and (iii) biodiesel testing on the diesel engine. These three stages were needed in designing and scaling-up the process tools and the process operation commercially. The reactive distillation process tools were designed and manufactured with reference to the design system tower by Kitzer, et.al. (2008). The manufactured reactive distillation consisted of packing distillation columns equipped with a reboiler and condenser, with the prototype made of stainless steel material equipped with sigh glass. The filling column expands the contact of liquid-vapor phase so that the two reactants between methanol and oil would be converted into methyl ester and glycerol. The initial results of the study indicated that the relatively good condition is reached at the peak temperature and the base of the column of 62°C and 71°C with NaOH 2% of methanol weight as the catalyst at the feed ratio of methanol and the sunan pecan oil 4:1. The result of the performance test of the diesel engine indicated that the efficiency of the biodiesel fuel was achieved relatively good at 1.7% with 2500 rpm engine speed.

The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

PubMed

Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

2014-03-01

In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

Stereospecific analysis of loxoprofen in plasma by chiral column liquid chromatography with a circular dichroism-based detector.

PubMed

Kanazawa, Hideko; Tsubayashi, Akane; Nagata, Yoshiko; Matsushima, Yoshikazu; Mori, Chiharu; Kizu, Junko; Higaki, Megumu

2002-03-01

The chiral separation of loxoprofen was achieved on a chiral column with UV and circular dichroism (CD) detection. The good resolution of four loxoprofen stereoisomers was obtained. The column used for the chiral separation was Chiralcel OJ column (250 x 4.6 mm) using hexane-2-propanol-trifluoroacetic acid (95:5:0.1), as an eluent. The flow-rate was 1.0 ml/min and the detection was at 225 nm. In addition, CD and UV spectra were obtained by stopped flow scanning. The method allows the determination of the stereoisomers of loxoprofen in human plasma after the administration of therapeutic dose of the racemic drug, thus HPLC with CD detector is useful for the stereospecific determination of loxoprofen products in biological samples.

Rapid separation and purification of uranium and plutonium from dilute-matrix samples

DOE PAGES

Armstrong, Christopher R.; Ticknor, Brian W.; Hall, Gregory; ...

2014-03-11

This work presents a streamlined separation and purification approach for trace uranium and plutonium from dilute (carrier-free) matrices. The method, effective for nanogram quantities of U and femtogram to picogram quantities of Pu, is ideally suited for environmental swipe samples that contain a small amount of collected bulk material. As such, it may be applicable for processing swipe samples such as those collected in IAEA inspection activities as well as swipes that are loaded with unknown analytes, such as those implemented in interlaboratory round-robin or proficiency tests. Additionally, the simplified actinide separation could find use in internal laboratory monitoring ofmore » clean room conditions prior to or following more extensive chemical processing. We describe key modifications to conventional techniques that result in a relatively rapid, cost-effective, and efficient U and Pu separation process. We demonstrate the efficacy of implementing anion exchange chromatography in a single column approach. We also show that hydrobromic acid is an effective substitute in lieu of hydroiodoic acid for eluting Pu. Lastly, we show that nitric acid is an effective digestion agent in lieu of perchloric acid and/or hydrofluoric acid. A step by step procedure of this process is detailed.« less

Preparation and retention mechanism study of graphene and graphene oxide bonded silica microspheres as stationary phases for high performance liquid chromatography.

PubMed

Zhang, Xiaoqiong; Chen, Sha; Han, Qiang; Ding, Mingyu

2013-09-13

Graphene oxide (GO) bonded stationary phase for high performance liquid chromatography (HPLC) was fabricated by coating GO sheets onto aminosilica microspheres via covalent coupling. Graphene (G) functionalized HPLC stationary phase was then prepared through hydrazine reduction of GO bonded silica (GO@SiO2) composite, which was the first example of using graphene as stationary-phase component for HPLC. Effective separations of the tested neutral and polar compounds on both GO@SiO2 and graphene bonded silica (G@SiO2) columns were achieved under the optimal experimental conditions. Compared with commercial C18 column, the different chromatographic performances of GO and graphene bonded columns were ascribed to their unique retention mechanisms. The polyaromatic scaffold of GO and graphene gives π-π stacking property and hydrophobic effect, and other retention mechanisms, such as π-π electron-donor-acceptor (EDA) interaction for the separation of nitroaromatic compounds and hydrogen bonding for hydroxyl and amino compounds, may also be taken into consideration. Experimental results indicated that the mixed-mode retention mechanism can facilitate the separation of analytes with similar hydrophobicity, which is a unique property compared with C18 column. Additionally, G@SiO2 showed higher affinity to aromatic analytes in contrast with GO@SiO2 and its retention mechanism was not consistent with the typical reversed phase behavior. The separation of aromatic compounds on G@SiO2 column relies primarily on the π-π stacking interaction and then the hydrophobicity, while the two interactions have equal shares on GO@SiO2 column. Copyright © 2013 Elsevier B.V. All rights reserved.

Capillary electrochromatographic separation of peptides using a macrocyclic polyamine for molecular recognition.

PubMed

Chen, Tse-Hsien; Misra, Tarun Kumar; Liu, Chuen-Ying

2008-04-01

A macrocyclic polyamine, 1,5,9,13,17,21,25,29-octaazacyclodotriacontane ([32]ane-N(8)), in the bonded phase was employed as a molecular receptor for CEC separation of oligopeptides. Parameters affecting the performance of the separations were considered. Baseline separation for the mixture of angiotensin I, angiotensin II, [Sar(1), Thr(8)]-angiotensin II, beta-casomorphin bovine, beta-casomorphin human, oxytocin acetate, tocinoic acid, vasopressin, and FMRF amide could be achieved using phosphate buffer (30 mM, pH 7) as the mobile phase. Column efficiency with average theoretical plate numbers of 69 000 plates/m and RSDs of <1% (n = 6) was achieved. [Met(5)]-enkephalin and [Leu(5)]-enkephalin, which have identical pI values and similar masses could be completely separated using acetate buffer (30 mM) with pH gradient (pH 3 inlet side and pH 4 outlet side). The results suggest that the mechanism for the peptide separation was mediated by a combination of electrophoretic migration and chromatographic retention involving anion coordination and anion exchange. After long-term use, the deviation of the EOF of the column after more than 600 injections was still within 6.0% of that for a freshly prepared column.

Nanotechnology and chip level systems for pressure driven liquid chromatography and emerging analytical separation techniques: a review.

PubMed

Lavrik, N V; Taylor, L T; Sepaniak, M J

2011-05-23

Pressure driven liquid chromatography (LC) is a powerful and versatile separation technique particularly suitable for differentiating species present in extremely small quantities. This paper briefly reviews main historical trends and focuses on more recently developed technological approaches in miniaturization and on-chip integration of LC columns. The review emphasizes enabling technologies as well as main technological challenges specific to pressure driven separations and highlights emerging concepts that could ultimately overcome fundamental limitations of conventional LC columns. Copyright © 2011 Elsevier B.V. All rights reserved.

In-situ polymerized PLOT columns III: divinylbenzene copolymers and dimethacrylate homopolymers

NASA Technical Reports Server (NTRS)

Shen, T. C.; Fong, M. M.

1994-01-01

Studies of divinylbenzene copolymers and dimethacrylate homopolymers indicate that the polymer pore size controls the separation of water and ammonia on porous-layer-open-tubular (PLOT) columns. To a lesser degree, the polarity of the polymers also affects the separation of a water-ammonia gas mixture. Our results demonstrate that the pore size can be regulated by controlling the cross-linking density or the chain length between the cross-linking functional groups. An optimum pore size will provide the best separation of water and ammonia.

Emulsion stability measurements by single electrode capacitance probe (SeCaP) technology

NASA Astrophysics Data System (ADS)

Schüller, R. B.; Løkra, S.; Salas-Bringas, C.; Egelandsdal, B.; Engebretsen, B.

2008-08-01

This paper describes a new and novel method for the determination of the stability of emulsions. The method is based on the single electrode capacitance technology (SeCaP). A measuring system consisting of eight individual measuring cells, each with a volume of approximately 10 ml, is described in detail. The system has been tested on an emulsion system based on whey proteins (WPC80), oil and water. Xanthan was added to modify the emulsion stability. The results show that the new measuring system is able to quantify the stability of the emulsion in terms of a differential variable. The whole separation process is observed much faster in the SeCaP system than in a conventional separation column. The complete separation process observed visually over 30 h is seen in less than 1.4 h in the SeCaP system.

Comprehensive analysis of pharmaceutical products using simultaneous mixed-mode (ion-exchange/reversed-phase) and hydrophilic interaction liquid chromatography.

PubMed

Kazarian, Artaches A; Nesterenko, Pavel N; Soisungnoen, Phimpha; Burakham, Rodjana; Srijaranai, Supalax; Paull, Brett

2014-08-01

Liquid chromatographic assays were developed using a mixed-mode column coupled in sequence with a hydrophilic interaction liquid chromatography column to allow the simultaneous comprehensive analysis of inorganic/organic anions and cations, active pharmaceutical ingredients, and excipients (carbohydrates). The approach utilized dual sample injection and valve-mediated column switching and was based upon a single high-performance liquid chromatography gradient pump. The separation consisted of three distinct sequential separation mechanisms, namely, (i) ion-exchange, (ii) mixed-mode interactions under an applied dual gradient (reversed-phase/ion-exchange), and (iii) hydrophilic interaction chromatography. Upon first injection, the Scherzo SS C18 column (Imtakt) provided resolution of inorganic anions and cations under isocratic conditions, followed by a dual organic/salt gradient to elute active pharmaceutical ingredients and their respective organic counterions and potential degradants. At the top of the mixed-mode gradient (high acetonitrile content), the mobile phase flow was switched to a preconditioned hydrophilic interaction liquid chromatography column, and the standard/sample was reinjected for the separation of hydrophilic carbohydrates, some of which are commonly known excipients in drug formulations. The approach afforded reproducible separation and resolution of up to 23 chemically diverse solutes in a single run. The method was applied to investigate the composition of commercial cough syrups (Robitussin®), allowing resolution and determination of inorganic ions, active pharmaceutical ingredients, excipients, and numerous well-resolved unknown peaks. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2009-08-01

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

High-throughput determination of faropenem in human plasma and urine by on-line solid-phase extraction coupled to high-performance liquid chromatography with UV detection and its application to the pharmacokinetic study.

PubMed

Xie, Rui; Wen, Jun; Wei, Hua; Fan, Guorong; Zhang, Dabing

2010-05-01

An automated system using on-line solid-phase extraction and HPLC with UV detection was developed for the determination of faropenem in human plasma and urine. Analytical process was performed isocratically with two reversed-phase columns connected by a switching valve. After simple pretreatment for plasma and urine with acetonitrile, a volume of 100microl upper layer of the plasma or urine samples was injected for on-line SPE column switching HPLC-UV analysis. The analytes were retained on the self-made trap column (Lichrospher C(18), 4.6mmx37mm, 25microm) with the loading solvent (20mM NaH(2)PO(4) adjusted pH 3.5) at flow rate of 2mlmin(-1), and most matrix materials were removed from the column to waste. After 0.5min washing, the valve was switched to another position so that the target analytes could be eluted from trap column to analytical column in the back-flush mode by the mobile phase (acetonitrile-20mM NaH(2)PO(4) adjusted pH 3.5, 16:84, v/v) at flow rate of 1.5mlmin(-1), and then separated on the analytical column (Ultimate XB-C(18), 4.6mmx50mm, 5microm).The complete cycle of the on-line SPE preconcentration purification and HPLC separation of the analytes was 5min. Calibration curves with good linearities (r=0.9994 for plasma sample and r=0.9988 for urine sample) were obtained in the range 0.02-5microgml(-1) in plasma and 0.05-10microg ml(-1) in urine for faropenem. The optimized method showed good performance in terms of specificity, linearity, detection and quantification limits, precision and accuracy. The method was successfully utilized to quantify faropenem in human plasma and urine to support the clinical pharmacokinetic studies. Copyright 2009 Elsevier B.V. All rights reserved.

Method and apparatus for the selective separation of gaseous coal gasification products by pressure swing adsorption

DOEpatents

Ghate, M.R.; Yang, R.T.

1985-10-03

Bulk separation of the gaseous components of multi-component gases provided by the gasification of coal including hydrogen, carbon monoxide, methane, and acid gases (carbon dioxide plus hydrogen sulfide) are selectively adsorbed by a pressure swing adsorption technique using activated carbon zeolite or a combination thereof as the adsorbent. By charging a column containing the adsorbent with a gas mixture and pressurizing the column to a pressure sufficient to cause the adsorption of the gases and then reducing the partial pressure of the contents of the column, the gases are selectively and sequentially desorbed. Hydrogen, the least absorbable gas of the gaseous mixture, is the first gas to be desorbed and is removed from the column in a co-current direction followed by the carbon monoxide, hydrogen and methane. With the pressure in the column reduced to about atmospheric pressure the column is evacuated in a countercurrent direction to remove the acid gases from the column. The present invention is particularly advantageous as a producer of high purity hydrogen from gaseous products of coal gasification and as an acid gas scrubber. 2 figs., 2 tabs.

Validation of an HPLC method for the determination of fleroxacin and its photo-degradation products in pharmaceutical forms.

PubMed

Djurdjevic, Predrag; Laban, Aleksandra; Jelikic-Stankov, Milena

2004-01-01

HPLC determination of fleroxacin in dosage forms was carried out using either reversed-phase column YMC pack ODS-AQ or Supelco LC Hisep shielded hydrophobic phase column, with UV detection at 280 nm. The mobile phase for ODS column consisted of 50:50:0.5 v/v/v and for Hisep column 15:85:0.5 v/v/v acetonitrile-water-triethylamine. The pH of the mobile phase was adjusted to 6.30 for ODS column and to 6.85 for Hisep column, with H3PO4. Linear response was obtained in the concentration range of fleroxacin between 0.01 and 1.30 micrograms/mL. Detection limit was 4.8 ng/mL. Recovery test in the determination of fleroxacin in "Quinodis" tablets (Hoffmann La Roche, nominal mass 400 or 200 mg) was 98-101% for both columns. The effect of the composition and pH of the mobile phase on spectra, retention time and dissociation constants of fleroxacin was discussed. The proposed method could be also used for separation of the photo-degradation products of fleroxacin. Ten degradation products were separated on the ODS-AQ column, thus confirming the suitability of the proposed method for stability study of fleroxacin in pharmaceuticals.

Microfluidic integration of parallel solid-phase liquid chromatography.

PubMed

Huft, Jens; Haynes, Charles A; Hansen, Carl L

2013-03-05

We report the development of a fully integrated microfluidic chromatography system based on a recently developed column geometry that allows for robust packing of high-performance separation columns in poly(dimethylsiloxane) microfluidic devices having integrated valves made by multilayer soft lithography (MSL). The combination of parallel high-performance separation columns and on-chip plumbing was used to achieve a fully integrated system for on-chip chromatography, including all steps of automated sample loading, programmable gradient generation, separation, fluorescent detection, and sample recovery. We demonstrate this system in the separation of fluorescently labeled DNA and parallel purification of reverse transcription polymerase chain reaction (RT-PCR) amplified variable regions of mouse immunoglobulin genes using a strong anion exchange (AEX) resin. Parallel sample recovery in an immiscible oil stream offers the advantage of low sample dilution and high recovery rates. The ability to perform nucleic acid size selection and recovery on subnanogram samples of DNA holds promise for on-chip genomics applications including sequencing library preparation, cloning, and sample fractionation for diagnostics.

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

PubMed

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

2017-01-01

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

Separation of sunscreens in skincare creams using greener high-temperature liquid chromatography and subcritical water chromatography.

PubMed

Kapalavavi, B; Marple, R; Gamsky, C; Yang, Y

2012-04-01

In this study, high-temperature liquid chromatographic (HTLC) and subcritical water chromatographic (SBWC) separations of sunscreens contained in skincare creams were achieved at temperatures ranging from 90 to 250°C. The columns employed in this work include a ZirChrom-DiamondBond-C18, a XTerra MS C18 and a XBridge C18 column. The quantity of methanol consumed by the greener HTLC sunscreen methods developed in this project is significantly reduced although the HTLC separation at this stage is not as efficient as that achieved by traditional HPLC. SBWC separation of sunscreens was also achieved on the XTerra MS C18 and the XBridge C18 columns using pure water at 230-250°C. Methanol was eliminated in the SBWC methods developed in this study. © 2011 The Authors. ICS © 2011 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Enantiomeric resolution of five chiral pesticides on a Chiralpak IB-H column by SFC.

PubMed

Jin, Lixia; Gao, Weiliang; Yang, Huayun; Lin, Chunmian; Liu, Weiping

2011-10-01

The enantiomeric separations of five chiral pesticides, diclofopmethyl, 1; benalaxy, 2; acetofenate, 3; myclobutanil, 4; and difenoconazole, 5, were conducted on a Chiralpak IB-H column by a packed-column supercritical fluid chromatography (p-SFC). All compounds, except difenoconazole and myclobutanil, were well resolved within 10 min. As the mobile phase polarity decreased through changing the percentage and the type of alcohol modifiers in the supercritical carbon dioxide (CO(2)), the retention time, the separation factors, and the resolution increased. However, based on the retention time and the resolution, the optimized separations were obtained with the mobile phase containing 10% 2-propanol for diclofop-methyl 1; benalaxy, 2; myclobutanil, 4; difenoconazole, 5; and containing 3% 2-propanol for acetofenate, 3. The optimized separation temperature was at 35°C under the supercritical fluid condition. The π-π interactions and the hydrogen bonding interactions between Chiralpak IB-H CSP and the analytes might be the main chiral discriminations on enantioseparation of these five pesticides.

Teaching Separations: Why, What, When, and How?

ERIC Educational Resources Information Center

Wankat, Phillip C.

2001-01-01

Describes how and when to teach separation science to chemical engineering students. Separation science is important for industrial businesses involving the manufacture of adsorption systems, distillation columns, extractors, and other separation equipment and techniques. (Contains 13 references.) (YDS)

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.

Counter-current motion in counter-current chromatography.

PubMed

Ito, Yoichiro

2014-12-12

After the CCC2012 meeting, I have received an e-mail regarding the terminology of "Countercurrent Chromatography". It stated that the term "Countercurrent" is a misnomer, because its stationary phase is motionless in the column and that the method should be renamed as liquid-liquid separations or centrifugal separations. However, it was found that these names are already used for various other techniques as found via Google search. The term "Countercurrent Chromatography" was originally made after two preparative methods of Countercurrent distribution and liquid Chromatography, both having no countercurrent motion in the column. However, it is surprising to find that this F1 hybrid method "Countercurrent Chromatography" can clearly exhibit countercurrent motion within the separation column in both hydrodynamic and hydrostatic equilibrium systems. This justifies that "Countercurrent Chromatography" is a proper term for this chromatographic method. Published by Elsevier B.V.

Triazine herbicide imprinted monolithic column for capillary electrochromatography.

PubMed

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

2015-12-01

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

Fabrication of powdery polymer aerogel as the stationary phase for high-resolution gas chromatographic separation.

PubMed

Zheng, Juan; Lu, Cuiming; Huang, Junlong; Chen, Luyi; Ni, Chuyi; Xie, Xintong; Zhu, Fang; Wu, Dingcai; Ouyang, Gangfeng

2018-08-15

Novel powdery polymer aerogel (PPA) prepared via the (micro)emulsion polymerization and the following hyper crosslinking reaction was fabricated as stationary phase of capillary column for the first time. Due to its powdery morphology, unique 3D nano-network structure, high surface area and good thermostability, the PPA-coated capillary column demonstrated high-resolution chromatographic separation towards nonpolar and weakly polar organic compounds, including benzene series, n-alkanes, ketone mixtures and trichlorobenzenes. Moreover, the reproducibility, quantitative analysis ability and thermostability of PPA-coated capillary column were also evaluated. The relative standard deviations for three replicate determinations of selected analytes were 0.02-0.11%, 0.12-0.26% and 1.2-3.6% for run-to-run, day-to-day and column-to-column analyses, respectively. The PPA demonstrated good thermostability, and the PPA-coated capillary column was proved to be heat-resistant (270 °C). The results of this study show PPA is an excellent candidate to be employed as stationary phase for gas chromatography capillary. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

Preparation of porous hollow silica spheres via a layer-by-layer process and the chromatographic performance

NASA Astrophysics Data System (ADS)

Wei, Xiaobing; Gong, Cairong; Chen, Xujuan; Fan, Guoliang; Xu, Xinhua

2017-03-01

Hollow silica spheres possessing excellent mechanical properties were successfully prepared through a layer-by-layer process using uniform polystyrene (PS) latex fabricated by dispersion polymerization as template. The formation of hollow SiO2 micro-spheres, structures and properties were observed in detail by zeta potential, SEM, TEM, FTIR, TGA and nitrogen sorption porosimetry. The results indicated that the hollow spheres were uniform with particle diameter of 1.6 μm and shell thickness of 150 nm. The surface area was 511 m2/g and the pore diameter was 8.36 nm. A new stationary phase for HPLC was obtained by using C18-derivatized hollow SiO2 micro-spheres as packing materials and the chromatographic properties were evaluated for the separation of some regular small molecules. The packed column showed low column pressure, high values of efficiency (up to about 43 000 plates/m) and appropriate asymmetry factors.

On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

PubMed

Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

2015-03-27

A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Microminiature gas chromatograph

DOEpatents

Yu, Conrad M.

1996-01-01

A microminiature gas chromatograph (.mu.GC) comprising a least one silicon wafer, a gas injector, a column, and a detector. The gas injector has a normally closed valve for introducing a mobile phase including a sample gas in a carrier gas. The valve is fully disposed in the silicon wafer(s). The column is a microcapillary in silicon crystal with a stationary phase and is mechanically connected to receive the mobile phase from the gas injector for the molecular separation of compounds in the sample gas. The detector is mechanically connected to the column for the analysis of the separated compounds of sample gas with electronic means, e.g., ion cell, field emitter and PIN diode.

Forward marching procedure for separated boundary-layer flows

NASA Technical Reports Server (NTRS)

Carter, J. E.; Wornom, S. F.

1975-01-01

A forward-marching procedure for separated boundary-layer flows which permits the rapid and accurate solution of flows of limited extent is presented. The streamwise convection of vorticity in the reversed flow region is neglected, and this approximation is incorporated into a previously developed (Carter, 1974) inverse boundary-layer procedure. The equations are solved by the Crank-Nicolson finite-difference scheme in which column iteration is carried out at each streamwise station. Instabilities encountered in the column iterations are removed by introducing timelike terms in the finite-difference equations. This provides both unconditional diagonal dominance and a column iterative scheme, found to be stable using the von Neumann stability analysis.

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

PubMed

Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2009-12-05

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

A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporous resin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry.

PubMed

Wang, Lu; Liu, Shu; Zhang, Xueju; Xing, Junpeng; Liu, Zhiqiang; Song, Fengrui

2016-06-24

In this paper, an analysis strategy integrating macroporous resin (AB-8) column chromatography and high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) combined with ion mobility spectrometry (IMS) was proposed and applied for identification and structural characterization of compounds from the fruits of Gardenia jasminoides. The extracts of G. jasminoides were separated by AB-8 resin column chromatography combined with reversed phase liquid chromatography (C18 column) and detected by electrospray ionization tandem mass spectrometry. Additionally, ion mobility spectrometry (IMS) was employed as a supplementary separation technique to discover previously undetected isomers from the fruits of G. jasminoides. A total of 71 compounds, including iridoids, flavonoids, triterpenes, monoterpenoids, carotenoids and phenolic acids were identified by the characteristic high resolution mass spectrometry and the ESI-MS/MS fragmentations. In conclusion, the IMS-MS technique achieved the separation of isomers in crocin-3 and crocin-4 according to their acquired mobility drift times differing from classical analysis by mass spectrometry. The proposed strategy can be used as a highly sensitive and efficient procedure for identification and separation isomeric components in extracts of herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

Highly hydrophilic and nonionic poly(2-vinyloxazoline)-grafted silica: a novel organic phase for high-selectivity hydrophilic interaction chromatography.

PubMed

Mallik, Abul K; Cheah, Wee Keat; Shingo, Kaori; Ejzaki, Aika; Takafuji, Makoto; Ihara, Hirotaka

2014-07-01

A new hydrophilic and nonionic poly(2-vinyloxazoline)-grafted silica (Sil-VOX(n)) phase was synthesized and applied for the separation of nucleosides and nucleobases in hydrophilic interaction chromatography (HILIC). Polymerization and immobilization onto silica were confirmed by using characterization techniques including (1)H NMR spectroscopy, elemental analysis, and diffuse reflectance infrared Fourier transform spectroscopy. The hydrophilicity or wettability of Sil-VOX(n) was observed by measuring the contact angle (59.9°). The chromatographic results were compared with those obtained with a conventional HILIC silica column. The Sil-VOX(n) phase showed much better separation of polar test analytes than the silica column, and the elution order was different. Differences in selectivity between these two columns indicate that the stationary phase cannot function merely as an inert support for a water layer into which the solutes are partitioned from the bulk mobile phase. To elucidate the interaction mechanism, the separation of dihydroxybenzene isomers was performed on both columns in normal-phase liquid chromatography. Sil-VOX(n) was very sensitive to the dipole moments of the positional isomers of polycyclic aromatic compounds in normal-phase liquid chromatography. The interaction mechanism for Sil-VOX(n) in HILIC separation is also described.

Preparation of diclofenac-imprinted polymer beads for selective molecular separation in water.

PubMed

Zhou, Tongchang; Kamra, Tripta; Ye, Lei

2018-03-01

Molecular imprinting technique is an attractive strategy to prepare materials for target recognition and rapid separation. In this work, a new type of diclofenac (DFC)-imprinted polymer beads was synthesized by Pickering emulsion polymerization using 2-(dimethylamino)ethyl methacrylate as the functional monomer. The selectivity and capacity of the molecularly imprinted polymers (MIPs) were investigated in aqueous solution. Equilibrium binding results show that the MIPs have a high selectivity to bind DFC in a wide range of pH values. Moreover, in liquid chromatography experiment, the imprinted polymer beads were packed into column to investigate the binding selectivity under nonequilibrium conditions. The retention time of DFC on the MIP column is significantly longer than its structural analogues. Also, retention of DFC on the MIP column was significantly longer than on the nonimprinted polymer column under aqueous condition. As the new MIP beads can be used to achieve direct separation of DFC from water, the synthetic method and the affinity beads developed in this work opened new possibilities for removing toxic chemicals from environmental and drinking water. Copyright © 2017 John Wiley & Sons, Ltd.

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.

Signal Enhancement in HPLC/Micro-Coil NMR Using Automated Column Trapping

PubMed Central

Djukovic, Danijel; Liu, Shuhui; Henry, Ian; Tobias, Brian; Raftery, Daniel

2008-01-01

A new HPLC-NMR system is described that performs analytical separation, pre-concentration, and NMR spectroscopy in rapid succession. The central component of our method is the online pre-concentration sequence that improves the match between post-column analyte peak volume and the micro-coil NMR detection volume. Separated samples are collected on to a C18 guard column with a mobile phase composed of 90% D2O/10% acetonitrile-D3, and back-flashed to the NMR micro-coil probe with 90% acetonitrile-D3/10% D2O. In order to assess the performance of our unit, we separated a standard mixture of 1 mM ibuprofen, naproxen, and phenylbutazone using a commercially available C18 analytical column. The S/N measurements from the NMR acquisitions indicated that we achieved signal enhancement factors up to 10.4 (±1.2)-fold. Furthermore, we observed that pre-concentration factors increased as the injected amount of analyte decreased. The highest concentration enrichment of 14.7 (±2.2)-fold was attained injecting 100 μL solution of 0.2 mM (~4 μg) ibuprofen. PMID:17037915

Tracing and separating plasma components causing matrix effects in hydrophilic interaction chromatography-electrospray ionization mass spectrometry.

PubMed

Ekdahl, Anja; Johansson, Maria C; Ahnoff, Martin

2013-04-01

Matrix effects on electrospray ionization were investigated for plasma samples analysed by hydrophilic interaction chromatography (HILIC) in gradient elution mode, and HILIC columns of different chemistries were tested for separation of plasma components and model analytes. By combining mass spectral data with post-column infusion traces, the following components of protein-precipitated plasma were identified and found to have significant effect on ionization: urea, creatinine, phosphocholine, lysophosphocholine, sphingomyelin, sodium ion, chloride ion, choline and proline betaine. The observed effect on ionization was both matrix-component and analyte dependent. The separation of identified plasma components and model analytes on eight columns was compared, using pair-wise linear correlation analysis and principal component analysis (PCA). Large changes in selectivity could be obtained by change of column, while smaller changes were seen when the mobile phase buffer was changed from ammonium formate pH 3.0 to ammonium acetate pH 4.5. While results from PCA and linear correlation analysis were largely in accord, linear correlation analysis was judged to be more straight-forward in terms of conduction and interpretation.

Oak ridge national laboratory automated clean chemistry for bulk analysis of environmental swipe samples

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

Bostick, Debra A.; Hexel, Cole R.; Ticknor, Brian W.

2016-11-01

To shorten the lengthy and costly manual chemical purification procedures, sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment. This addresses a serious need in the nuclear safeguards community to debottleneck the separation of U and Pu in environmental samples—currently performed by overburdened chemists—with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on current COTS equipment that was modified for U/Pu separations utilizing Eichrom™ TEVA and UTEVA resins. Initial verification of individual columns yielded small elution volumes with consistent elution profiles and good recovery. Combined columnmore » calibration demonstrated ample separation without crosscontamination of the eluent. Automated packing and unpacking of the built-in columns initially showed >15% deviation in resin loading by weight, which can lead to inconsistent separations. Optimization of the packing and unpacking methods led to a reduction in the variability of the packed resin to less than 5% daily. The reproducibility of the automated system was tested with samples containing 30 ng U and 15 pg Pu, which were separated in a series with alternating reagent blanks. These experiments showed very good washout of both the resin and the sample from the columns as evidenced by low blank values. Analysis of the major and minor isotope ratios for U and Pu provided values well within data quality limits for the International Atomic Energy Agency. Additionally, system process blanks spiked with 233U and 244Pu tracers were separated using the automated system after it was moved outside of a clean room and yielded levels equivalent to clean room blanks, confirming that the system can produce high quality results without the need for expensive clean room infrastructure. Comparison of the amount of personnel time necessary for successful manual vs. automated chemical separations showed a significant decrease in hands-on time from 9.8 hours to 35 minutes for seven samples, respectively. This documented time savings and reduced labor translates to a significant cost savings per sample. Overall, the system will enable faster sample reporting times at reduced costs by limiting personnel hours dedicated to the chemical separation.« less

The non-modulated transfer of total effluent for serially coupled columns in gas chromatography.

PubMed

Krupcík, Ján; Mydlová-Memersheimerová, Janka; Májek, Pavel; Zapadlo, Michal; Sandra, Pat

2010-03-12

The non-modulated transfer (NMT) of the total effluent of the separation of polychlorinated biphenyls (PCBs) on two columns coupled in series has been studied. A non-polar poly(5%-phenyl-95%-methyl)siloxane column (40 m x 100 microm x 0.1 microm) and a polar 70%-cyanopropyl-polysilphenylene-siloxane column (4 m x 0.1 mm x 0.1 microm) were used as (1)D and (2)D columns, respectively. The effluents from both the (1)D column and the (1)D+(2)D column series were monitored independently by two FIDs. Data from the (1)D and (1)D+(2)D integration reports were used to evaluate the NMT experiment. (1)D retention times, t(R,i,D1), were directly accessible from (1)D integration report while (2)D retention times, t(R,i,B), were calculated for all corresponding peak pairs from (1)D and (1)D+(2)D integration reports as a difference t(R,i,D2)=t(R,i,D1+D2)-t(R,i,D1). Search for corresponding peaks of PCB congeners in the (1)D and (1)D+(2)D chromatograms is elucidated in detail on standard PCB samples and on PCB congeners present in the technical formulation Arochlor 1242. Both retention times (t(R,i,D1) and t(R,i,D2)) as well as peak widths at half height (w(h,i)) and peak heights (h(i)) obtained from integration reports were used to construct 2D and 3D images for PCB NMT separations on serially coupled columns. The performance of the NMT procedure is illustrated by the separation of (i) standard PCB solutions, (ii) a mixture of the 209 PCBs, and (iii) a mixture of Arochlor 1242 and hydrocarbons on the DB-5+BPX-70 column series. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Combined Pressure, Temperature Contrast and Surface-Enhanced Separation of Carbon Dioxide for Post-Combustion Carbon Capture

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

Wang, Zhen; Wong, Michael; Gupta, Mayank

The Rice University research team developed a hybrid carbon dioxide (CO 2) absorption process combining absorber and stripper columns using a high surface area ceramic foam gas-liquid contactor for enhanced mass transfer and utilizing waste heat for regeneration. This integrated absorber/desorber arrangement will reduce space requirements, an important factor for retrofitting existing coal-fired power plants with CO 2 capture technology. Described in this report, we performed an initial analysis to estimate the technical and economic feasibility of the process. A one-dimensional (1D) CO 2 absorption column was fabricated to measure the hydrodynamic and mass transfer characteristics of the ceramic foam.more » A bench-scale prototype was constructed to implement the complete CO 2 separation process and tested to study various aspects of fluid flow in the process. A model was developed to simulate the two-dimensional (2D) fluid flow and optimize the CO 2 capture process. Test results were used to develop a final technoeconomic analysis and identify the most appropriate absorbent as well as optimum operating conditions to minimize capital and operating costs. Finally, a technoeconomic study was performed to assess the feasibility of integrating the process into a 600 megawatt electric (MWe) coal-fired power plant. With process optimization, $82/MWh of COE can be achieved using our integrated absorber/desorber CO 2 capture technology, which is very close to DOE's target that no more than a 35% increase in COE with CCS. An environmental, health, and safety (EH&S) assessment of the capture process indicated no significant concern in terms of EH&S effects or legislative compliance.« less

Demonstration of motionless Knudsen pump based micro-gas chromatography featuring micro-fabricated columns and on-column detectors.

PubMed

Liu, Jing; Gupta, Naveen K; Wise, Kensall D; Gianchandani, Yogesh B; Fan, Xudong

2011-10-21

This paper reports the investigation of a micro-gas chromatography (μGC) system that utilizes an array of miniaturized motionless Knudsen pumps (KPs) as well as microfabricated separation columns and optical detectors. A prototype system was built to achieve a flow rate of 1 mL min(-1) and 0.26 mL min(-1) for helium and dry air, respectively, when they were used as carrier gas. This system was then employed to evaluate GC performance compromises and demonstrate the ability to separate and detect gas mixtures containing analytes of different volatilities and polarities. Furthermore, the use of pressure programming of the KP array was demonstrated to significantly shorten the analysis time while maintaining a high detection resolution. Using this method, we obtained a high resolution detection of 5 alkanes of different volatilities within 5 min. Finally, we successfully detected gas mixtures of various polarities using a tandem-column μGC configuration by installing two on-column optical detectors to obtain complementary chromatograms.

Column-coupling strategies for multidimensional electrophoretic separation techniques.

PubMed

Kler, Pablo A; Sydes, Daniel; Huhn, Carolin

2015-01-01

Multidimensional electrophoretic separations represent one of the most common strategies for dealing with the analysis of complex samples. In recent years we have been witnessing the explosive growth of separation techniques for the analysis of complex samples in applications ranging from life sciences to industry. In this sense, electrophoretic separations offer several strategic advantages such as excellent separation efficiency, different methods with a broad range of separation mechanisms, and low liquid consumption generating less waste effluents and lower costs per analysis, among others. Despite their impressive separation efficiency, multidimensional electrophoretic separations present some drawbacks that have delayed their extensive use: the volumes of the columns, and consequently of the injected sample, are significantly smaller compared to other analytical techniques, thus the coupling interfaces between two separations components must be very efficient in terms of providing geometrical precision with low dead volume. Likewise, very sensitive detection systems are required. Additionally, in electrophoretic separation techniques, the surface properties of the columns play a fundamental role for electroosmosis as well as the unwanted adsorption of proteins or other complex biomolecules. In this sense the requirements for an efficient coupling for electrophoretic separation techniques involve several aspects related to microfluidics and physicochemical interactions of the electrolyte solutions and the solid capillary walls. It is interesting to see how these multidimensional electrophoretic separation techniques have been used jointly with different detection techniques, for intermediate detection as well as for final identification and quantification, particularly important in the case of mass spectrometry. In this work we present a critical review about the different strategies for coupling two or more electrophoretic separation techniques and the different intermediate and final detection methods implemented for such separations.

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.

Automated metal-free multiple-column nanoLC for improved phosphopeptide analysis sensitivity and throughput

PubMed Central

Zhao, Rui; Ding, Shi-Jian; Shen, Yufeng; Camp, David G.; Livesay, Eric A.; Udseth, Harold; Smith, Richard D.

2009-01-01

We report on the development and characterization of automated metal-free multiple-column nanoLC instrumentation for sensitive and high-throughput analysis of phosphopeptides with mass spectrometry analysis. The system implements a multiple-column capillary LC fluidic design developed for high-throughput analysis of peptides (Anal. Chem. 2001, 73, 3011–3021), incorporating modifications to achieve broad and sensitive analysis of phosphopeptides. The integrated nanoLC columns (50 µm i.d. × 30 cm containing 5 µm C18 particles) and the on-line solid phase extraction columns (150 µm i.d. × 4 cm containing 5 µm C18 particles) were connected to automatic switching valves with non-metal chromatographic accessories, and other modifications to avoid the exposure of the analyte to any metal surfaces during handling, separation, and electrospray ionization. The nanoLC developed provided a separation peak capacity of ∼250 for phosphopeptides (and ∼400 for normal peptides). A detection limit of 0.4 fmol was obtained when a linear ion trap tandem mass spectrometer (Finnegan LTQ) was coupled to a 50-µm i.d. column of the nanoLC. The separation power and sensitivity provided by the nanoLC-LTQ enabled identification of ∼4600 phosphopeptide candidates from ∼60 µg COS-7 cell tryptic digest followed by IMAC enrichment and ∼520 tyrosine phosphopeptides from ∼2 mg of human T cells digests followed by phosphotyrosine peptide immunoprecipitation. PMID:19217835

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

PubMed

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

2016-03-03

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

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.

Development of gas chromatography-flame ionization detection system with a single column and liquid nitrogen-free for measuring atmospheric C2-C12 hydrocarbons.

PubMed

Liu, Chengtang; Mu, Yujing; Zhang, Chenglong; Zhang, Zhibo; Zhang, Yuanyuan; Liu, Junfeng; Sheng, Jiujiang; Quan, Jiannong

2016-01-04

A liquid nitrogen-free GC-FID system equipped with a single column has been developed for measuring atmospheric C2-C12 hydrocarbons. The system is consisted of a cooling unit, a sampling unit and a separation unit. The cooling unit is used to meet the temperature needs of the sampling unit and the separation unit. The sampling unit includes a dehydration tube and an enrichment tube. No breakthrough of the hydrocarbons was detected when the temperature of the enrichment tube was kept at -90 °C and sampling volume was 400 mL. The separation unit is a small round oven attached on the cooling column. A single capillary column (OV-1, 30 m × 0.32 mm I.D.) was used to separate the hydrocarbons. An optimal program temperature (-60 ∼ 170 °C) of the oven was achieved to efficiently separate C2-C12 hydrocarbons. There were good linear correlations (R(2)=0.993-0.999) between the signals of the hydrocarbons and the enrichment amount of hydrocarbons, and the relative standard deviation (RSD) was less than 5%, and the method detection limits (MDLs) for the hydrocarbons were in the range of 0.02-0.10 ppbv for sampling volume of 400 mL. Field measurements were also conducted and more than 50 hydrocarbons from C2 to C12 were detected in Beijing city. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-08-01

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

An Automated Distillation Column for the Unit Operations Laboratory

ERIC Educational Resources Information Center

Perkins, Douglas M.; Bruce, David A.; Gooding, Charles H.; Butler, Justin T.

2005-01-01

A batch distillation apparatus has been designed and built for use in the undergraduate unit operations laboratory course. The column is fully automated and is accompanied by data acquisition and control software. A mixture of 1­-propanol and 2-­propanol is separated in the column, using either a constant distillate rate or constant composition…

A Better Method for Filling Pasteur Pipet Chromatography Columns

ERIC Educational Resources Information Center

Ruekberg, Ben

2006-01-01

An alternative method for the preparation of Pasteur pipet chromatography columns is presented that allows the column to be filled with solvent without bubbles and allows greater control of fluid flow while the materials to be separated are added. Students are required to wear gloves and goggles and caution should be used while handling glass…

Heat integrated ethanol dehydration flowsheets

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

Hutahaean, L.S.; Shen, W.H.; Brunt, V. Van

1995-04-01

zA theoretical evaluation of heat-integrated heterogeneous-azeotropic ethanol-water distillation flowsheets is presented. Simulations of two column flowsheets using several different hydrocarbon entrainers reveal a region of potential heat integration and substantial reduction in operating energy. In this paper, methods for comparing hydrocarbon entrainers are shown. Two aspects of entrainers are related to operating and capital costs. The binary azeotropic composition of the entrainer-ethanol mixture is related to the energy requirements of the flowsheet. A temperature difference in the azeotrophic column is related to the size of the column and overall process staging requirements. Although the hydrophobicity of an entrainer is essentialmore » for specification of staging in the dehydration column, no substantial increase in operating energy results from an entrainer that has a higher water content. Likewise, liquid-liquid equilibria between several entrainer-ethanol-water mixtures have no substantial effect on either staging or operation. Rather, increasing the alcohol content of the entrainer-ethanol azeotrope limits its recovery in the dehydration column, and increases the recycle and reflux streams. These effects both contribute to increasing the separation energy requirements and reducing the region of potential heat integration. A cost comparison with a multieffect extractive distillation flowsheet reveals that the costs are comparable; however, the extractive distillation flowsheet is more cost effective as operating costs increase.« less

Cation exchange concentraion of the Americium product from TRUEX

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

Barney, G.S.; Cooper, T.D.; Fisher, F.D.

1991-06-01

A transuranic extraction (TRUEX) process has been developed to separate and recover plutonium, americium, and other transuranic (TRU) elements from acid wastes. The main objective of the process is to reduce the effluent to below the TRU limit for actinide concentrations (<100 nCi/g of material) so it can be disposed of inexpensively. The process yields a dilute nitric acid stream containing low concentrations of the extracted americium product. This solution also contains residual plutonium and trace amounts of iron. The americium will be absorbed into a cation exchange resin bed to concentrate it for disposal or for future use. Themore » overall objective of these laboratory tests was to determine the performance of the cation exchange process under expected conditions of the TRUEX process. Effects of acid, iron, and americium concentrations on americium absorption on the resin were determined. Distribution coefficients for americium absorption from acide solutions on the resin were measured using batch equilibrations. Batch equilibrations were also used to measure americium absorption in the presence of complexants. This data will be used to identify complexants and solution conditions that can be used to elute the americium from the columns. The rate of absorption was measured by passing solutions containing americium through small columns of resin, varying the flowrates, and measuring the concentrations of americium in the effluent. The rate data will be used to estimate the minimum bed size of the columns required to concentrate the americium product. 11 refs. , 10 figs., 2 tabs.« less

Simulation of elution profiles in liquid chromatography - II: Investigation of injection volume overload under gradient elution conditions applied to second dimension separations in two-dimensional liquid chromatography.

PubMed

Stoll, Dwight R; Sajulga, Ray W; Voigt, Bryan N; Larson, Eli J; Jeong, Lena N; Rutan, Sarah C

2017-11-10

An important research direction in the continued development of two-dimensional liquid chromatography (2D-LC) is to improve the detection sensitivity of the method. This is especially important in applications where injection of large volumes of effluent from the first dimension ( 1 D) column into the second dimension ( 2 D) column leads to severe 2 D peak broadening and peak shape distortion. For example, this is common when coupling two reversed-phase columns and the organic solvent content of the 1 D mobile phase overwhelms the 2 D column with each injection of 1 D effluent, leading to low resolution in the second dimension. In a previous study we validated a simulation approach based on the Craig distribution model and adapted from the work of Czok and Guiochon [1] that enabled accurate simulation of simple isocratic and gradient separations with very small injection volumes, and isocratic separations with mismatched injection and mobile phase solvents [2]. In the present study we have extended this simulation approach to simulate separations relevant to 2D-LC. Specifically, we have focused on simulating 2 D separations where gradient elution conditions are used, there is mismatch between the sample solvent and the starting point in the gradient elution program, injection volumes approach or even exceed the dead volume of the 2 D column, and the extent of sample loop filling is varied. To validate this simulation we have compared results from simulations and experiments for 101 different conditions, including variation in injection volume (0.4-80μL), loop filling level (25-100%), and degree of mismatch between sample organic solvent and the starting point in the gradient elution program (-20 to +20% ACN). We find that that the simulation is accurate enough (median errors in retention time and peak width of -1.0 and -4.9%, without corrections for extra-column dispersion) to be useful in guiding optimization of 2D-LC separations. However, this requires that real injection profiles obtained from 2D-LC interface valves are used to simulate the introduction of samples into the 2 D column. These profiles are highly asymmetric - simulation using simple rectangular pulses leads to peak widths that are far too narrow under many conditions. We believe the simulation approach developed here will be useful for addressing practical questions in the development of 2D-LC methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation techniques: Chromatography

PubMed Central

Coskun, Ozlem

2016-01-01

Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

A GC-system for the analysis of residual geothermal gases

USGS Publications Warehouse

Sheppard, D.S.; Truesdell, A.H.

1985-01-01

The gases evolved from geothermal fields, after condensation of H2O, CO2, H2S and NH3 in caustic solution, contain He, H2, Ar, O2, N2, CH4 and higher hydrocarbons. The analysis for the major components in these residual gas mixtures can be achieved by use of two simple gas chromatographs in parallel, and using 5A?? molecular sieve. The separation of He and H2 to baseline is achieved by using low temperatures (30??C) coupled with a relatively long column; and the difficult separation of Ar and O2 is achieved by use of a cryogenically cooled column. The use of switching valves to backflush and bypass columns ensures that a minimum time for analysis can be achieved whilst retaining baseline separations of the He/H2 and Ar/O2 pairs. ?? 1985 Friedr. Vieweg & Sohn Verlagsgesellschaft mbH.

Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

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

Tan, H.

1999-03-31

The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performedmore » in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.« less

DEVELOPMENT OF A FABRICATION PROCESS FOR SOL-GEL/METAL HYDRIDE COMPOSITE GRANULES

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

Hansen, E; Eric Frickey, E; Leung Heung, L

An external gelation process was developed to produce spherical granules that contain metal hydride particles in a sol-gel matrix. Dimensionally stable granules containing metal hydrides are needed for applications such as hydrogen separation and hydrogen purification that require columns containing metal hydrides. Gases must readily flow through the metal hydride beds in the columns. Metal hydrides reversibly absorb and desorb hydrogen and hydrogen isotopes. This is accompanied by significant volume changes that cause the metal hydride to break apart or decrepitate. Repeated cycling results in very fine metal hydride particles that are difficult to handle and contain. Fine particles tendmore » to settle and pack making it more difficult to flow gases through a metal hydride bed. Furthermore, the metal hydrides can exert a significant force on the containment vessel as they expand. These problems associated with metal hydrides can be eliminated with the granulation process described in this report. Small agglomerates of metal hydride particles and abietic acid (a pore former) were produced and dispersed in a colloidal silica/water suspension to form the feed slurry. Fumed silica was added to increase the viscosity of the feed slurry which helped to keep the agglomerates in suspension. Drops of the feed slurry were injected into a 27-foot tall column of hot ({approx}70 C), medium viscosity ({approx}3000 centistokes) silicone oil. Water was slowly evaporated from the drops as they settled. The drops gelled and eventually solidified to form spherical granules. This process is referred to as external gelation. Testing was completed to optimize the design of the column, the feed system, the feed slurry composition, and the operating parameters of the column. The critical process parameters can be controlled resulting in a reproducible fabrication technique. The residual silicone oil on the surface of the granules was removed by washing in mineral spirits. The granules were dried in air at 40 C. The granules were heated to 230 C for 30 minutes in argon to remove the remaining water and organic materials. The resulting product was spherical composite granules (100 to 2000 micron diameter) with a porous silica matrix containing small agglomerates of metal hydride particles. Open porosity in the silica matrix allows hydrogen to permeate rapidly through the matrix but the pores are small enough to contain the metal hydride particles. Additional porosity around the metal hydride particles, induced using abietic acid as a pore former, allows the particles to freely expand and contract without fracturing the brittle sol-gel matrix. It was demonstrated that the granules readily absorb and desorb hydrogen while remaining integral and dimensionally stable. Microcracking was observed after the granules were cycled in hydrogen five times. The strength of the granules was improved by coating them with a thin layer of a micro-porous polymer sol-gel that would allow hydrogen to freely pass through the coating but would filter out metal hydride poisons such as water and carbon monoxide. It was demonstrated that if a thin sol-gel coating was applied after the granules were cycled, the coating not only improved the strength of the granules but the coated granules retained their strength after additional hydrogen cycling tests. This additional strength is needed to extend the lifetime of the granules and to survive the compressive load in a large column of granules. Additional hydrogen adsorption tests are planned to evaluate the performance of coated granules after one hundred cycles. Tests will also be performed to determine the effects of metal hydride poisons on the granules. The results of these tests will be documented in a separate report. The process that was developed to form these granules could be scaled to a production process. The process to form granules from a mixture of metal hydride particles and pore former such as abietic acid can be scaled up using commercial granulators. The current laboratory-scale external gelation column produces approximately one gram of granules per hour. To increase the production output from a single column, multiple feed injection systems in a larger diameter column could be used.« less

28. November 1969 CASTIRON DRAGON GROTESQUE BELOW BASE OF COLUMN ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

28. November 1969 CAST-IRON DRAGON GROTESQUE BELOW BASE OF COLUMN SEPARATING WINDOWS ON NORTH SIDE OF RIGGS LIBRARY - Georgetown University, Healy Building, Thirty-seventh & O Streets, Northwest, Washington, District of Columbia, DC

Desulfurization of coal by microbial column flotation.

PubMed

Ohmura, N; Saiki, H

1994-06-05

Twenty-three strains capable of oxidizing iron were isolated from coal and ore storage sites as well as coal and ore mines, volcanic areas, and hot spring. Four strains were found to have high iron-oxidizing activity. One strain (T-4) was selected for this experiment since the strain showed the fastest leaching rate of iron and sulfate from pyrite among the four strains. The T-4 strain was assigned for Thiobacillus ferrooxidans from its cultural and morphological characteristics.Bacterial treatment was applied to column flotation. An increase of cell density in the microbial column flotation resulted in the increase of pyrite removal from a coal-pyrite mixture (high sulfur imitated coal) with corresponding decrease of coal recovery. The addition of kerosene into the microbial column flotation increased the recovery of the imitated coal from 55% (without kerosene) to 81% (with 50 microL/L kerosene) with the reduction of pyrite sulfur content from 11% (feed coal) to 3.9% (product coal). The kerosene addition could reduce the pyritic sulfur content by collecting the coal in the recovery. However, the addition could not enhance separation of pyrite from the coal-pyrite mixture, since pyrite rejection was not affected by the increase of the kerosene addition. An excellent separation was obtained by the microbial flotation using a long column which had a length-diameter (L/D) ratio of 12.7. The long column flotation reduced the pyritic sulfur content from 11% (feed coal) to 1.8% (product coal) when 80% of the feed coal was recovered without the kerosene addition. The long column flotation not only attained an excellent separation but also reduced the amount of cells for desulfurization to as little as one-tenth of the reported amount.

A nitromethane-based HPLC system alternative to acetonitrile for carotenoid analysis of fruit and vegetables.

PubMed

Sandmann, Gerhard

2010-01-01

Acetonitrile-based HPLC systems are the most commonly used for carotenoid analysis from different plant tissues. Because of the acetonitrile shortage, an HPLC system for the separation of carotenoids on C(18) reversed-phase columns was developed in which an acetonitrile-alcohol-based mobile phase was replaced by nitromethane. This solvent comes closest to acetonitrile with respect to its elutrophic property. Our criterion was to obtain similar separation and retention times for a range of differently structured carotenoids. This was achieved by further increase in the lipophilicity with ethylacetate. For all the carotenoids which we tested, we found co-elution only of β-cryptoxanthin and lycopene. By addition of 1% of water, separation of this pair of carotenoids was also achieved. The final recommended mobile phase consisted of nitromethane : 2-propanol : ethyl acetate : water (79 : 10 : 10 : 1, by volume). On Nucleosil C(18) columns and related ones like Hypersil C(18), we obtained separation of carotenes, hydroxyl, epoxy and keto derivatives, which resembles the excellent separation properties of acetonitrile-based mobile phases on C(18) reversed phase columns. We successfully applied the newly developed HPLC system to the separation of carotenoids from different vegetables and fruit. Copyright © 2010 John Wiley & Sons, Ltd.

Development of a 45kpsi ultrahigh pressure liquid chromatography instrument for gradient separations of peptides using long microcapillary columns and sub-2μm particles.

PubMed

Grinias, Kaitlin M; Godinho, Justin M; Franklin, Edward G; Stobaugh, Jordan T; Jorgenson, James W

2016-10-21

Commercial chromatographic instrumentation for bottom-up proteomics is often inadequate to resolve the number of peptides in many samples. This has inspired a number of complex approaches to increase peak capacity, including various multidimensional approaches, and reliance on advancements in mass spectrometry. One-dimensional reversed phase separations are limited by the pressure capabilities of commercial instruments and prevent the realization of greater separation power in terms of speed and resolution inherent to smaller sorbents and ultrahigh pressure liquid chromatography. Many applications with complex samples could benefit from the increased separation performance of long capillary columns packed with sub-2μm sorbents. Here, we introduce a system that operates at a constant pressure and is capable of separations at pressures up to 45kpsi. The system consists of a commercially available capillary liquid chromatography instrument, for sample management and gradient creation, and is modified with a storage loop and isolated pneumatic amplifier pump for elevated separation pressure. The system's performance is assessed with a complex peptide mixture and a range of microcapillary columns packed with sub-2μm C18 particles. Copyright © 2016 Elsevier B.V. All rights reserved.

Enantioselective Analytical- and Preparative-Scale Separation of Hexabromocyclododecane Stereoisomers Using Packed Column Supercritical Fluid Chromatography.

PubMed

Riddell, Nicole; Mullin, Lauren Gayle; van Bavel, Bert; Ericson Jogsten, Ingrid; McAlees, Alan; Brazeau, Allison; Synnott, Scott; Lough, Alan; McCrindle, Robert; Chittim, Brock

2016-11-10

Hexabromocyclododecane (HBCDD) is an additive brominated flame retardant which has been listed in Annex A of the Stockholm Convention for elimination of production and use. It has been reported to persist in the environment and has the potential for enantiomer-specific degradation, accumulation, or both, making enantioselective analyses increasingly important. The six main stereoisomers of technical HBCDD (i.e., the (+) and (-) enantiomers of α-, β-, and γ-HBCDD) were separated and isolated for the first time using enantioselective packed column supercritical fluid chromatography (pSFC) separation methods on a preparative scale. Characterization was completed using published chiral liquid chromatography (LC) methods and elution profiles, as well as X-ray crystallography, and the isolated fractions were definitively identified. Additionally, the resolution of the enantiomers, along with two minor components of the technical product (δ- and ε-HBCDD), was investigated on an analytical scale using both LC and pSFC separation techniques, and changes in elution order were highlighted. Baseline separation of all HBCDD enantiomers was achieved by pSFC on an analytical scale using a cellulose-based column. The described method emphasizes the potential associated with pSFC as a green method of isolating and analyzing environmental contaminants of concern.

Preparative isolation of alkaloids from Dactylicapnos scandens using pH-zone-refining counter-current chromatography by changing the length of the separation column.

PubMed

Wang, Xiao; Dong, Hongjing; Yang, Bin; Liu, Dahui; Duan, Wenjuan; Huang, Luqi

2011-12-01

pH-Zone-refining counter-current chromatography was successfully applied for the preparative separation of alkaloids from Dactylicapnos scandens. The two-phase solvent system was composed of petroleum ether-ethyl acetate-methanol-water (3:7:1:9, v/v), where 20 mM of triethylamine (TEA) was added to the upper phase as a retainer and 5 mM of hydrochloric acid (HCl) to the aqueous phase as an eluter. In this experiment, the apparatus with an adjustable length of the separation column was used for the separation of alkaloids from D. scandens and the resolution of the compounds can be remarkably improved by increasing the length of the separation column. As a result, 70 mg protopin, 30 mg (+) corydine, 120 mg (+) isocorydine and 40 mg (+) glaucine were obtained from 1.0 g of the crude extracts and each with 99.2%, 96.5%, 99.3%, 99.5% purity as determined by HPLC. The chemical structures of these compounds were confirmed by positive ESI-MS and (1)H NMR. Copyright © 2011 Elsevier B.V. All rights reserved.

Gravity separation of fat, somatic cells, and bacteria in raw and pasteurized milks.

PubMed

Caplan, Z; Melilli, C; Barbano, D M

2013-04-01

The objective of experiment 1 was to determine if the extent of gravity separation of milk fat, bacteria, and somatic cells is influenced by the time and temperature of gravity separation or the level of contaminating bacteria present in the raw milk. The objective of experiment 2 was to determine if different temperatures of milk heat treatment affected the gravity separation of milk fat, bacteria, and somatic cells. In raw milk, fat, bacteria, and somatic cells rose to the top of columns during gravity separation. About 50 to 80% of the fat and bacteria were present in the top 8% of the milk after gravity separation of raw milk. Gravity separation for 7h at 12°C or for 22h at 4°C produced equivalent separation of fat, bacteria, and somatic cells. The completeness of gravity separation of fat was influenced by the level of bacteria in the milk before separation. Milk with a high bacterial count had less (about 50 to 55%) gravity separation of fat than milk with low bacteria count (about 80%) in 22h at 4°C. Gravity separation caused fat, bacteria, and somatic cells to rise to the top of columns for raw whole milk and high temperature, short-time pasteurized (72.6°C, 25s) whole milk. Pasteurization at ≥76.9°C for 25s prevented all 3 components from rising, possibly due to denaturation of native bovine immunoglobulins that normally associate with fat, bacteria, and somatic cells during gravity separation. Gravity separation can be used to produce reduced-fat milk with decreased bacterial and somatic cell counts, and may be a critical factor in the history of safe and unique traditional Italian hard cheeses produced from gravity-separated raw milk. A better understanding of the mechanism of this natural process could lead to the development of new nonthermal thermal technology (that does not involve heating the milk to high temperatures) to remove bacteria and spores from milk or other liquids. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

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.

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

PubMed

Park, Sin Young; Cheong, Won Jo

2016-05-01

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

Supramolecular separation mechanism of pentafluorophenyl column using ibuprofen and omeprazole as markers: LC-MS and simulation study.

PubMed

Hussain, Afzal; AlAjmi, Mohamed F; Ali, Imran

2018-06-01

The pentafluorophenyl (PFP) column is emerging as a new advancement in separation science to analyze a wide range of analytes and, thus, its separation mechanism at supramolecular level is significant. We developed a mechanism for the separation of ibuprofen and omeprazole using different combinations (ranging from 50:50 to 60:40) of water-acetonitrile containing 0.1% formic acid as the mobile phase. The column used was Waters Acquity UPLC HSS PFP (75 × 2.1 mm, 1.8 μm). The reverse order of elution was observed in different combinations of the mobile phases. The docking study indicated hydrogen bonding between ibuprofen and PFP stationary phase (binding energy was -11.30 kJ/mol). Separation at PFP stationary phase is controlled by hydrogen bonding along with π-π interactions. This stationary phase may be used to analyze both aromatic and aliphatic analytes. The developed mechanism will be useful to separate various analytes by considering the possible interactions, leading to saving of energy, time and money. In addition, this work will be highly useful in preparative chromatography where separation is the major problem at a large scale. Moreover, the developed LC-MS-QTOF method may be used to analyze ibuprofen and omeprazole in an unknown sample owing to the low value of detection limits. Copyright © 2018 John Wiley & Sons, Ltd.

Microminiature gas chromatograph

DOEpatents

Yu, C.M.

1996-12-10

A microminiature gas chromatograph ({mu}GC) comprising a least one silicon wafer, a gas injector, a column, and a detector. The gas injector has a normally closed valve for introducing a mobile phase including a sample gas in a carrier gas. The valve is fully disposed in the silicon wafer(s). The column is a microcapillary in silicon crystal with a stationary phase and is mechanically connected to receive the mobile phase from the gas injector for the molecular separation of compounds in the sample gas. The detector is mechanically connected to the column for the analysis of the separated compounds of sample gas with electronic means, e.g., ion cell, field emitter and PIN diode. 7 figs.

3D-liquid chromatography as a complex mixture characterization tool for knowledge-based downstream process development.

PubMed

Hanke, Alexander T; Tsintavi, Eleni; Ramirez Vazquez, Maria Del Pilar; van der Wielen, Luuk A M; Verhaert, Peter D E M; Eppink, Michel H M; van de Sandt, Emile J A X; Ottens, Marcel

2016-09-01

Knowledge-based development of chromatographic separation processes requires efficient techniques to determine the physicochemical properties of the product and the impurities to be removed. These characterization techniques are usually divided into approaches that determine molecular properties, such as charge, hydrophobicity and size, or molecular interactions with auxiliary materials, commonly in the form of adsorption isotherms. In this study we demonstrate the application of a three-dimensional liquid chromatography approach to a clarified cell homogenate containing a therapeutic enzyme. Each separation dimension determines a molecular property relevant to the chromatographic behavior of each component. Matching of the peaks across the different separation dimensions and against a high-resolution reference chromatogram allows to assign the determined parameters to pseudo-components, allowing to determine the most promising technique for the removal of each impurity. More detailed process design using mechanistic models requires isotherm parameters. For this purpose, the second dimension consists of multiple linear gradient separations on columns in a high-throughput screening compatible format, that allow regression of isotherm parameters with an average standard error of 8%. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:1283-1291, 2016. © 2016 American Institute of Chemical Engineers.

Composite silicon nanostructure arrays fabricated on optical fibre by chemical etching of multicrystal silicon film.

PubMed

Zuo, Zewen; Zhu, Kai; Ning, Lixin; Cui, Guanglei; Qu, Jun; Huang, Wanxia; Shi, Yi; Liu, Hong

2015-04-17

Integrating nanostructures onto optical fibers presents a promising strategy for developing new-fashioned devices and extending the scope of nanodevices' applications. Here we report the first fabrication of a composite silicon nanostructure on an optical fiber. Through direct chemical etching using an H2O2/HF solution, multicrystal silicon films with columnar microstructures are etched into a vertically aligned, inverted-cone-like nanorod array embedded in a nanocone array. A faster dissolution rate of the silicon at the void-rich boundary regions between the columns is found to be responsible for the separation of the columns, and thus the formation of the nanostructure array. The morphology of the nanorods primarily depends on the microstructure of the columns in the film. Through controlling the microstructure of the as-grown film and the etching parameters, the structural control of the nanostructure is promising. This fabrication method can be extended to a larger length scale, and it even allows roll-to-roll processing.

Removal of furan and phenolic compounds from simulated biomass hydrolysates by batch adsorption and continuous fixed-bed column adsorption methods.

PubMed

Lee, Sang Cheol; Park, Sunkyu

2016-09-01

It has been proposed to remove all potential inhibitors and sulfuric acid in biomass hydrolysates generated from dilute-acid pretreatment of biomass, based on three steps of sugar purification process. This study focused on its first step in which furan and phenolic compounds were selectively removed from the simulated hydrolysates using activated charcoal. Batch adsorption experiments demonstrated that the affinity of activated charcoal for each component was highest in the order of vanillic acid, 4-hydroxybenzoic acid, furfural, acetic acid, sulfuric acid, and xylose. The affinity of activated charcoal for furan and phenolic compounds proved to be significantly higher than that of the other three components. Four separation strategies were conducted with a combination of batch adsorption and continuous fixed-bed column adsorption methods. It was observed that xylose loss was negligible with near complete removal of furan and phenolic compounds, when at least one fixed-bed column adsorption was implemented in the strategy. Copyright © 2016 Elsevier Ltd. All rights reserved.

Optimation and Determination of Fe-Oxinate Complex by Using High Performance Liquid Chromatography

NASA Astrophysics Data System (ADS)

Oktavia, B.; Nasra, E.; Sary, R. C.

2018-04-01

The need for iron will improve the industrial processes that require iron as its raw material. Control of industrial iron waste is very important to do. One method of iron analysis is to conduct indirect analysis of iron (III) ions by complexing with 8-Hydroxyquinoline or oxine. In this research, qualitative and quantitative tests of iron (III) ions in the form of complex with oxine. The analysis was performed using HPLC at a wavelength of 470 nm with an ODS C18 column. Three methods of analysis were performed: 1) Fe-oxinate complexes were prepared in an ethanol solvent so no need for separation anymore, (2) Fe-oxinate complexes were made in chloroform so that a solvent extraction was required before the complex was injected into the column while the third complex was formed in the column, wherein the eluent contains the oxide and the metal ions are then injected. The resulting chromatogram shows that the 3rd way provides a better chromatogram for iron analysis.

Fast gradient screening of pharmaceuticals with 5 cm long, narrow bore reversed-phase columns packed with sub-3 μm core-shell and sub-2 μm totally porous particles.

PubMed

Fekete, Szabolcs; Fekete, Jeno

2011-04-15

The performance of 5 cm long narrow-bore columns packed with 2.6-2.7 μm core-shell particles and a column packed with 1.7 μm totally porous particles was compared in very fast gradient separations of polar neutral active pharmaceutical compounds. Peak capacities as a function of flow-rate and gradient time were measured. Peak capacities around 160-170 could be achieved within 25 min with these 5 cm long columns. The highest peak capacity was obtained with the Kinetex column however it was found that as the flow-rate increases, the peak capacity of the new Poroshell-120 column is getting closer to that obtained with the Kinetex column. Considering the column permeability, peak capacity per unit time and per unit pressure was also calculated. In this comparison the advantage of sub-3 μm core-shell particles is more significant compared to sub-2 μm totally porous particles. Moreover it was found that the very similar sized (d(p)=2.7 μm) and structured (ρ=0.63) new Poroshell-120 and the earlier introduced Ascentis Express particles showed different efficiency. Results obtained showed that the 5 cm long narrow bore columns packed with sub-3 μm core-shell particles offer the chance of very fast and efficient gradient separations, thus these columns can be applied for fast screening measurements of routine pharmaceutical analysis such as cleaning validation. Copyright © 2011 Elsevier B.V. All rights reserved.

Zwitterionic chiral stationary phases based on cinchona and chiral sulfonic acids for the direct stereoselective separation of amino acids and other amphoteric compounds.

PubMed

Zhang, Tong; Holder, Emilie; Franco, Pilar; Lindner, Wolfgang

2014-06-01

An extensive series of free amino acids and analogs were directly resolved into enantiomers (and stereoisomers where appropriate) by HPLC on zwitterionic chiral stationary phases (Chiralpak ZWIX(+) and Chiralpak ZWIX(-)). The interaction and chiral recognition mechanisms were based on the synergistic double ion-paring process between the analyte and the chiral selectors. The chiral separation and elution order were found to be predictable for primary α-amino acids with apolar aliphatic side chains. A systematic investigation was undertaken to gain an insight into the influence of the structural features on the enantiorecognition. The presence of polar and/or aromatic groups in the analyte structure is believed to tune the double ion-paring equilibrium by the involvement of the secondary interaction forces such as hydrogen bonding, Van der Waals forces and π-π stacking in concert with steric parameters. The ZWIX chiral columns were able to separate enantiomers and stereoisomers of various amphoteric compounds with no need for precolumn derivatization. Column switching between ZWIX(+) and ZWIX(-) is believed to be an instrumental tool to reverse or control the enantiomers elution order, due to the complementarity of the applied chiral selectors. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid sequential determination of Pu, 90Sr and 241Am nuclides in environmental samples using an anion exchange and Sr-Spec resins.

PubMed

Lee, M H; Ahn, H J; Park, J H; Park, Y J; Song, K

2011-02-01

This paper presents a quantitative and rapid method of sequential separation of Pu, (90)Sr and (241)Am nuclides in environmental soil samples with an anion exchange resin and Sr Spec resin. After the sample solution was passed through an anion exchange column connected to a Sr Spec column, Pu isotopes were purified from the anion exchange column. Strontium-90 was separated from other interfering elements by the Sr Spec column. Americium-241 was purified from lanthanides by the anion exchange resin after oxalate co-precipitation. Measurement of Pu and Am isotopes was carried out using an α-spectrometer. Strontium-90 was measured by a low-level liquid scintillation counter. The radiochemical procedure of Pu, (90)Sr and (241)Am nuclides investigated in this study validated by application to IAEA reference materials and environmental soil samples. Copyright © 2010 Elsevier Ltd. All rights reserved.

A novel octadecylsilane functionalized graphene oxide/silica composite stationary phase for high performance liquid chromatography.

PubMed

Liang, Xiaojing; Wang, Shuai; Liu, Shujuan; Liu, Xia; Jiang, Shengxiang

2012-08-01

An octadecylsilane functionalized graphene oxide/silica stationary phase was fabricated by assembling graphene oxide onto the silica particles through an amide bond and subsequent immobilization of octadecylsilane. The chromatographic properties of the stationary phase were investigated by reversed-phase chromatography with alkylbenzenes, polycyclic aromatic hydrocarbons, amines, and phenolic compounds as the analytes. All the compounds achieved good separation on the column. The comparison between a C18 commercial column and the new stationary phase indicated that the existence of π-electron system of graphene oxide allows π-π interaction between analyte and octadecylsilane functionalized graphene oxide/silica stationary phase except for hydrophobic interaction, while only hydrophobic interaction presented between analyte and C18 commercial column. This suggests that some analytes can be better separated on the octadecylsilane functionalized graphene oxide/silica column. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Non-planar microfabricated gas chromatography column

DOEpatents

Lewis, Patrick R.; Wheeler, David R.

2007-09-25

A non-planar microfabricated gas chromatography column comprises a planar substrate having a plurality of through holes, a top lid and a bottom lid bonded to opposite surfaces of the planar substrate, and inlet and outlet ports for injection of a sample gas and elution of separated analytes. A plurality of such planar substrates can be aligned and stacked to provide a longer column length having a small footprint. Furthermore, two or more separate channels can enable multi-channel or multi-dimensional gas chromatography. The through holes preferably have a circular cross section and can be coated with a stationary phase material or packed with a porous packing material. Importantly, uniform stationary phase coatings can be obtained and band broadening can be minimized with the circular channels. A heating or cooling element can be disposed on at least one of the lids to enable temperature programming of the column.

Mobile phase effects on the retention on polar columns with special attention to the dual hydrophilic interaction-reversed-phase liquid chromatography mechanism, a review.

PubMed

Jandera, Pavel; Hájek, Tomáš

2018-01-01

Hydrophilic interaction liquid chromatography on polar columns in aqueous-organic mobile phases has become increasingly popular for the separation of many biologically important compounds in chemical, environmental, food, toxicological, and other samples. In spite of many new applications appearing in literature, the retention mechanism is still controversial. This review addresses recent progress in understanding of the retention models in hydrophilic interaction liquid chromatography. The main attention is focused on the role of water, both adsorbed by the column and contained in the bulk mobile phase. Further, the theoretical retention models in the isocratic and gradient elution modes are discussed. The dual hydrophilic interaction liquid chromatography reversed-phase retention mechanism on polar columns is treated in detail, especially with respect to the practical use in one- and two-dimensional liquid chromatography separations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High Throughput Strontium Isotope Method for Monitoring Fluid Flow Related to Geological CO2 Storage

NASA Astrophysics Data System (ADS)

Capo, R. C.; Wall, A. J.; Stewart, B. W.; Phan, T. T.; Jain, J. C.; Hakala, J. A.; Guthrie, G. D.

2012-12-01

Natural isotope tracers, such as strontium (Sr), can be a unique and powerful component of a monitoring strategy at a CO2 storage site, facilitating both the quantification of reaction progress for fluid-rock interactions and the tracking of brine migration caused by CO2 injection. Several challenges must be overcome, however, to enable the routine use of isotopic tracers, including the ability to rapidly analyze numerous aqueous samples with potentially complex chemical compositions. In a field situation, it might be necessary to analyze tens of samples over a short period of time to identify subsurface reactions and respond to unexpected fluid movement in the host formation. These conditions require streamlined Sr separation chemistry for samples ranging from pristine groundwaters to those containing high total dissolved solids, followed by rapid measurement of isotope ratios with high analytical precision. We have optimized Sr separation chemistry and MC-ICP-MS methods to provide rapid and precise measurements of isotope ratios in geologic, hydrologic, and environmental samples. These improvements will allow an operator to independently prepare samples for Sr isotope analysis off-site using fast, low cost chemical separation procedures and commercially available components. Existing vacuum-assisted Sr separation procedures were modified by using inexpensive disposable parts to eliminate cross contamination. Experimental results indicate that the modified columns provide excellent separation of Sr from chemically complex samples and that Sr can be effectively isolated from problematic matrix elements (e.g., Ca, Ba, K) associated with oilfield brines and formation waters. The separation procedure is designed for high sample throughput in which batches of 24 samples can be processed in approximately 2 hours, and are ready for Sr isotope measurements by MC-ICP-MS immediately after collection from the columns. Precise Sr isotope results can be achieved by MC-ICP-MS with a throughput of 4 to 5 samples per hour. Our mean measured value of NIST Sr isotope standard SRM 987 is 0.710265 ± 0.000014 (2σ, n = 94). A range of brines and CO2-rich fluids analyzed by this method yielded results within the analytical uncertainty of 87Sr/86Sr ratios previously determined by standard column separation and thermal ionization mass spectrometry. This method provides a fast and effective way to use Sr isotopes for monitoring purposes related to geological CO2 storage.

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.

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.

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

PubMed

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

2010-06-01

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

A high-throughput, simultaneous analysis of carotenoids, chlorophylls and tocopherol using sub two micron core shell technology columns.

PubMed

Chebrolu, Kranthi K; Yousef, Gad G; Park, Ryan; Tanimura, Yoshinori; Brown, Allan F

2015-09-15

A high-throughput, robust and reliable method for simultaneous analysis of five carotenoids, four chlorophylls and one tocopherol was developed for rapid screening large sample populations to facilitate molecular biology and plant breeding. Separation was achieved for 10 known analytes and four unknown carotenoids in a significantly reduced run time of 10min. Identity of the 10 analytes was confirmed by their UV-Vis absorption spectras. Quantification of tocopherol, carotenoids and chlorophylls was performed at 290nm, 460nm and 650nm respectively. In this report, two sub two micron particle core-shell columns, Kinetex from Phenomenex (1.7μm particle size, 12% carbon load) and Cortecs from Waters (1.6μm particle size, 6.6% carbon load) were investigated and their separation efficiencies were evaluated. The peak resolutions were >1.5 for all analytes except for chlorophyll-a' with Cortecs column. The ruggedness of this method was evaluated in two identical but separate instruments that produced CV<2 in peak retentions for nine out of 10 analytes separated. Copyright © 2015 Elsevier B.V. All rights reserved.

Selective liquid chromatographic separation of yttrium from heavier rare earth elements using acetic acid as a novel eluent.

PubMed

Kifle, Dejene; Wibetoe, Grethe

2013-09-13

One of the major difficulties in the rare earth elements separation is purification of yttrium from heavy rare earth elements. Thus, an HPLC method using acetic acid as novel eluent was explored for selective separation of yttrium form the heavy rare earth elements. When acetic acid is used as a mobile phase yttrium eluted with the lighter lanthanides. This is contrary to its relative position amongst heavier lanthanides when eluents commonly used for separation of rare earth elements were employed. The shift in elution position of yttrium with acetic acid as eluent may reflect a relatively lower stability constant of the yttrium-AcOH complex (in the same order as for the lighter lanthanides) compared to the corresponding AcOH complexes with heavy lanthanides, enabling selective separation of yttrium from the latter. The method was successfully used for selective separation of yttrium in mixed rare earth sample containing about 80% of yttrium and about 20% of heavy rare earth oxides. Thus, the use of AcOH as eluent is an effective approach for separating and determining the trace amounts of heavy rare earth elements in large amounts of yttrium matrix. Separation was performed on C18 column by running appropriate elution programs. The effluent from the column was monitored with diode array detector at absorbance wavelength of 658nm after post column derivatization with Arsenazo III. Copyright © 2013 Elsevier B.V. All rights reserved.

Properties of Two-Variety Natural Luffa Sponge Columns as Potential Mattress Filling Materials

PubMed Central

Chen, Yuxia; Zhang, Kaiting; Yuan, Fangcheng; Zhang, Tingting; Weng, Beibei; Wu, Shanshan; Huang, Aiyue; Su, Na; Guo, Yong

2018-01-01

Luffa sponge (LS) is a resourceful material with fibro-vascular reticulated structure and extremely high porosity, which make it a potential candidate for manufacturing light mattress. In this study, two types of LS columns, namely high-density (HD) and low-density (LD) columns, were investigated as materials for filling the mattress. The results showed that the compressive strength of HD LS columns was significantly greater than that of LD LS columns. However, the densification strains of the two types of LS column were both in the range of 0.6 to 0.7. Besides, HD LS columns separately pressed to the smooth plateau region and the initial densification region exhibited a partial recovery of instant height when they were unloaded, and then both of them showed no more than 4.2% of height recovery after being allowed to rest at a constant temperature and humidity for 24 h. In contrast, when LD LS columns were compressed to the smooth plateau region, the height recovery was less than 1.62% compared to when they were pressed to the initial densification region, and that was more than 15.62%. Similar to other plant fibers used as mattress fillers, the two types of LS columns also showed good water absorption capacity—both of them could absorb water from as much as 2.07 to 3.45 times their own weight. At the same time, the two types of LS columns also showed good water desorption. The water desorption ratio of HD and LD LS columns separately reached 76.86 and 91.44%, respectively, after being let rest at a constant temperature and humidity for 13 h. PMID:29614744

Derringer desirability and kinetic plot LC-column comparison approach for MS-compatible lipopeptide analysis.

PubMed

D'Hondt, Matthias; Verbeke, Frederick; Stalmans, Sofie; Gevaert, Bert; Wynendaele, Evelien; De Spiegeleer, Bart

2014-06-01

Lipopeptides are currently re-emerging as an interesting subgroup in the peptide research field, having historical applications as antibacterial and antifungal agents and new potential applications as antiviral, antitumor, immune-modulating and cell-penetrating compounds. However, due to their specific structure, chromatographic analysis often requires special buffer systems or the use of trifluoroacetic acid, limiting mass spectrometry detection. Therefore, we used a traditional aqueous/acetonitrile based gradient system, containing 0.1% (m/v) formic acid, to separate four pharmaceutically relevant lipopeptides (polymyxin B 1 , caspofungin, daptomycin and gramicidin A 1 ), which were selected based upon hierarchical cluster analysis (HCA) and principal component analysis (PCA). In total, the performance of four different C18 columns, including one UPLC column, were evaluated using two parallel approaches. First, a Derringer desirability function was used, whereby six single and multiple chromatographic response values were rescaled into one overall D -value per column. Using this approach, the YMC Pack Pro C18 column was ranked as the best column for general MS-compatible lipopeptide separation. Secondly, the kinetic plot approach was used to compare the different columns at different flow rate ranges. As the optimal kinetic column performance is obtained at its maximal pressure, the length elongation factor λ ( P max / P exp ) was used to transform the obtained experimental data (retention times and peak capacities) and construct kinetic performance limit (KPL) curves, allowing a direct visual and unbiased comparison of the selected columns, whereby the YMC Triart C18 UPLC and ACE C18 columns performed as best. Finally, differences in column performance and the (dis)advantages of both approaches are discussed.

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

PubMed

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

2013-09-01

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

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

PubMed

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

2006-11-17

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

Separation of 103Ru from a proton irradiated thorium matrix: A potential source of Auger therapy radionuclide 103mRh

DOE PAGES

Mastren, Tara; Radchenko, Valery; Hopkins, Philip D.; ...

2017-12-22

Ruthenium-103 is the parent isotope of 103mRh (t1/2 56.1 min), an isotope of interest for Auger electron therapy. During the proton irradiation of thorium targets, large amounts of 103Ru are generated through proton induced fission. Furthermore, the development of a two part chemical separation process to isolate 103Ru in high yield and purity from a proton irradiated thorium matrix on an analytical scale is described herein. The first part employed an anion exchange column to remove cationic actinide/lanthanide impurities along with the majority of the transition metal fission products. Secondly, an extraction chromatographic column utilizing diglycolamide functional groups was usedmore » to decontaminate 103Ru from the remaining impurities. This method then resulted in a final radiochemical yield of 83 ± 5% of 103Ru with a purity of 99.9%. Additionally, measured nuclear reaction cross sections for the formation of 103Ru and 106Ru via the 232Th(p,f) 103,106Ru reactions are reported within.« less

Chaotropic salts in liquid chromatographic method development for the determination of pramipexole and its impurities following quality-by-design principles.

PubMed

Vemić, Ana; Rakić, Tijana; Malenović, Anđelija; Medenica, Mirjana

2015-01-01

The aim of this paper is to present a development of liquid chromatographic method when chaotropic salts are used as mobile phase additives following the QbD principles. The effect of critical process parameters (column chemistry, salt nature and concentration, acetonitrile content and column temperature) on the critical quality attributes (retention of the first and last eluting peak and separation of the critical peak pairs) was studied applying the design of experiments-design space methodology (DoE-DS). D-optimal design is chosen in order to simultaneously examine both categorical and numerical factors in minimal number of experiments. Two ways for the achievement of quality assurance were performed and compared. Namely, the uncertainty originating from the models was assessed by Monte Carlo simulations propagating the error equal to the variance of the model residuals and propagating the error originating from the model coefficients' calculation. The baseline separation of pramipexole and its five impurities is achieved fulfilling all the required criteria while the method validation proved its reliability. Copyright © 2014 Elsevier B.V. All rights reserved.

Separation of 103Ru from a proton irradiated thorium matrix: A potential source of Auger therapy radionuclide 103mRh

PubMed Central

Hopkins, Philip D.; Engle, Jonathan W.; Weidner, John W.; Copping, Roy; Brugh, Mark; Nortier, F. Meiring; Birnbaum, Eva R.; John, Kevin D.

2017-01-01

Ruthenium-103 is the parent isotope of 103mRh (t1/2 56.1 min), an isotope of interest for Auger electron therapy. During the proton irradiation of thorium targets, large amounts of 103Ru are generated through proton induced fission. The development of a two part chemical separation process to isolate 103Ru in high yield and purity from a proton irradiated thorium matrix on an analytical scale is described herein. The first part employed an anion exchange column to remove cationic actinide/lanthanide impurities along with the majority of the transition metal fission products. Secondly, an extraction chromatographic column utilizing diglycolamide functional groups was used to decontaminate 103Ru from the remaining impurities. This method resulted in a final radiochemical yield of 83 ± 5% of 103Ru with a purity of 99.9%. Additionally, measured nuclear reaction cross sections for the formation of 103Ru and 106Ru via the 232Th(p,f)103,106Ru reactions are reported within. PMID:29272318

Analysis of multiple quaternary ammonium compounds in the brain using tandem capillary column separation and high resolution mass spectrometric detection.

PubMed

Falasca, Sara; Petruzziello, Filomena; Kretz, Robert; Rainer, Gregor; Zhang, Xiaozhe

2012-06-08

Endogenous quaternary ammonium compounds are involved in various physiological processes in the central nervous system. In the present study, eleven quaternary ammonium compounds, including acetylcholine, choline, carnitine, acetylcarnitine and seven other acylcarnitines of low polarity, were analyzed from brain extracts using a two dimension capillary liquid chromatography-Fourier transform mass spectrometry method. To deal with their large difference in hydrophobicities, tandem coupling between reversed phase and hydrophilic interaction chromatography columns was used to separate all the targeted quaternary ammonium compounds. Using high accuracy mass spectrometry in selected ion monitoring mode, all the compounds could be detected from each brain sample with high selectivity. The developed method was applied for the relative quantification of these quaternary ammonium compounds in three different brain regions of tree shrews: prefrontal cortex, striatum, and hippocampus. The comparative analysis showed that quaternary ammonium compounds were differentially distributed across the three brain areas. The analytical method proved to be highly sensitive and reliable for simultaneous determination of all the targeted analytes from brain samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Standing wave design and optimization of a simulated moving bed chromatography for separation of xylobiose and xylose under the constraints on product concentration and pressure drop.

PubMed

Lee, Chung-Gi; Choi, Jae-Hwan; Park, Chanhun; Wang, Nien-Hwa Linda; Mun, Sungyong

2017-12-08

The feasibility of a simulated moving bed (SMB) technology for the continuous separation of high-purity xylobiose (X2) from the output of a β-xylosidase X1→X2 reaction has recently been confirmed. To ensure high economical efficiency of the X2 production method based on the use of xylose (X1) as a starting material, it is essential to accomplish the comprehensive optimization of the X2-separation SMB process in such a way that its X2 productivity can be maximized while maintaining the X2 product concentration from the SMB as high as possible in consideration of a subsequent lyophilization step. To address this issue, a suitable SMB optimization tool for the aforementioned task was prepared based on standing wave design theory. The prepared tool was then used to optimize the SMB operation parameters, column configuration, total column number, adsorbent particle size, and X2 yield while meeting the constraints on X2 purity, X2 product concentration, and pressure drop. The results showed that the use of a larger particle size caused the productivity to be limited by the constraint on X2 product concentration, and a maximum productivity was attained by choosing the particle size such that the effect of the X2-concentration limiting factor could be balanced with that of pressure-drop limiting factor. If the target level of X2 product concentration was elevated, higher productivity could be achieved by decreasing particle size, raising the level of X2 yield, and increasing the column number in the zones containing the front and rear of X2 solute band. Copyright © 2017 Elsevier B.V. All rights reserved.

Quantitative structure-retention relationship models for the prediction of the reversed-phase HPLC gradient retention based on the heuristic method and support vector machine.

PubMed

Du, Hongying; Wang, Jie; Yao, Xiaojun; Hu, Zhide

2009-01-01

The heuristic method (HM) and support vector machine (SVM) were used to construct quantitative structure-retention relationship models by a series of compounds to predict the gradient retention times of reversed-phase high-performance liquid chromatography (HPLC) in three different columns. The aims of this investigation were to predict the retention times of multifarious compounds, to find the main properties of the three columns, and to indicate the theory of separation procedures. In our method, we correlated the retention times of many diverse structural analytes in three columns (Symmetry C18, Chromolith, and SG-MIX) with their representative molecular descriptors, calculated from the molecular structures alone. HM was used to select the most important molecular descriptors and build linear regression models. Furthermore, non-linear regression models were built using the SVM method; the performance of the SVM models were better than that of the HM models, and the prediction results were in good agreement with the experimental values. This paper could give some insights into the factors that were likely to govern the gradient retention process of the three investigated HPLC columns, which could theoretically supervise the practical experiment.

The study on the extraction method of indirubin from Indigo Naturalis.

PubMed

Cheng, Li-hui

2007-01-01

To discuss how to extract the indirubin of the higher purity from Indigo Naturalis. After extracting the indirubin from Indigo Naturalis by acetic ether, compare the separation effect of the extract in Si gel column with that in alumina column. The indirubin in Indigo Naturalis by Si gel column chromatography is chosen. The purity of indirubin is 98.3% after Si gel column chromatography. The indiruhbin of the higher purity was attained by the simple experimental method.

Preparative electrophoresis with on-column optical fiber monitoring and direct elution into a minimized volume.

PubMed

Jackson, George W; Willson, Richard

2005-11-01

A "column-format" preparative electrophoresis device which obviates the need for gel extraction or secondary electro-elution steps is described. Separated biomolecules are continuously detected and eluted directly into a minimal volume of free solution for subsequent use. An optical fiber allows the species of interest to be detected just prior to elution from the gel column, and a small collection volume is created by addition of an ion-exchange membrane near the end of the column.

Enantiomeric separation of volatile organics by gas chromatography for the in situ analysis of extraterrestrial materials: kinetics and thermodynamics investigation of various chiral stationary phases.

PubMed

Freissinet, C; Buch, A; Szopa, C; Sternberg, R

2013-09-06

The performances of several commercial chiral capillary columns have been evaluated with the aim of determining the one most suitable for enantiomeric separation in a gas chromatograph onboard a space probe. We compared the GC-MS response of three capillary columns coated with different chiral stationary phases (CSP) using volatile chiral organic molecules which are potential markers of a prebiotic organic chemistry. The three different chiral capillary columns are Chirasil-Val, with an amino acid derivative CSP, ChiralDex-β-PM, with a CSP composed of dissolved permethylated β-cyclodextrins in polysiloxane, and Chirasil-Dex, with a CSP made of modified cyclodextrins chemically bonded to the polysiloxane backbone. Both kinetics and thermodynamics studies have been carried out to evaluate the chiral recognition potential in these different types of columns. The thermodynamic parameters also allow a better understanding of the driving forces affecting the retention and separation of the enantiomers. The Chirasil-Dex-CSP displays the best characteristics for an optimal resolution of the chiral compounds, without preliminary derivatization. This CSP had been chosen to be the only chiral column in the Sample Analysis at Mars (SAM) experiment onboard the current Mars Science Laboratory (MSL) mission, and is also part of the Mars Organic Molecules Analyzer (MOMA) gas chromatograph onboard the next Martian mission ExoMars. The use of this column could also be extended to all space missions aimed at studying chirality in space. Copyright © 2013 Elsevier B.V. All rights reserved.

Spiral Countercurrent Chromatography

PubMed Central

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

2013-01-01

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

Establishment of a search library about benzylisoquinoline alkaloids based on selective separation on the binaphthyl column and standard analysis on C18 column.

PubMed

Liu, Qiaoxia; Zhou, Binbin; Wang, Xinliang; Ke, Yanxiong; Jin, Yu; Yin, Lihui; Liang, Xinmiao

2012-12-01

A search library about benzylisoquinoline alkaloids was established based on preparation of alkaloid fractions from Rhizoma coptidis, Cortex phellodendri, and Rhizoma corydalis. In this work, two alkaloid fractions from each herbal medicine were first prepared based on selective separation on the "click" binaphthyl column. And then these alkaloid fractions were analyzed on C18 column by liquid chromatography coupled with tandem mass spectrometry. Many structure-related compounds were included in these alkaloids fractions, which led to easy separation and good MS response in further work. Therefore, a search library of 52 benzylisoquinoline alkaloids was established, which included eight aporphine, 19 tetrahydroprotoberberine, two protopine, two benzyltetrahydroisoquinoline, and 21 protoberberine alkaloids. The information of the search library contained compound names, structures, retention times, accurate masses, fragmentation pathways of benzylisoquionline alkaloids, and their sources from three herbal medicines. Using such a library, the alkaloids, especially those trace and unknown components in some herbal medicine could be accurately and quickly identified. In addition, the distribution of benzylisoquinoline alkaloids in the herbal medicines could be also summarized by searching the source samples in the library. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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.

Low energy consumption method for separating gaseous mixtures and in particular for medium purity oxygen production

DOEpatents

Jujasz, Albert J.; Burkhart, James A.; Greenberg, Ralph

1988-01-01

A method for the separation of gaseous mixtures such as air and for producing medium purity oxygen, comprising compressing the gaseous mixture in a first compressor to about 3.9-4.1 atmospheres pressure, passing said compressed gaseous mixture in heat exchange relationship with sub-ambient temperature gaseous nitrogen, dividing the cooled, pressurized gaseous mixture into first and second streams, introducing the first stream into the high pressure chamber of a double rectification column, separating the gaseous mixture in the rectification column into a liquid oxygen-enriched stream and a gaseous nitrogen stream and supplying the gaseous nitrogen stream for cooling the compressed gaseous mixture, removing the liquid oxygen-enriched stream from the low pressure chamber of the rectification column and pumping the liquid, oxygen-enriched steam to a predetermined pressure, cooling the second stream, condensing the cooled second stream and evaporating the oxygen-enriched stream in an evaporator-condenser, delivering the condensed second stream to the high pressure chamber of the rectification column, and heating the oxygen-enriched stream and blending the oxygen-enriched stream with a compressed blend-air stream to the desired oxygen concentration.

An alternative procedure for uranium analysis in drinking water using AQUALIX columns: application to varied French bottled waters.

PubMed

Bouvier-Capely, C; Bonthonneau, J P; Dadache, E; Rebière, F

2014-01-01

The general population is chronically exposed to uranium ((234)U, (235)U, and (238)U) and polonium ((210)Po) mainly through day-to-day food and beverage intake. The measurement of these naturally-occurring radionuclides in drinking water is important to assess their health impact. In this work the applicability of calix[6]arene-derivatives columns for uranium analysis in drinking water was investigated. A simple and effective method was proposed on a specific column called AQUALIX, for the separation and preconcentration of U from drinking water. This procedure is suitable for routine analysis and the analysis time is considerably shortened (around 4h) by combining the separation on AQUALIX with fast ICP-MS measurement. This new method was tested on different French bottled waters (still mineral water, sparkling mineral water, and spring water). Then, the case of simultaneous presence of uranium and polonium in water was considered due to interferences in alpha spectrometry measurement. A protocol was proposed using a first usual step of spontaneous deposition of polonium on silver disc in order to separate Po, followed by the uranium extraction on AQUALIX column before alpha spectrometry counting. © 2013 Published by Elsevier B.V.

Preparation of convection interaction media isobutyl disc monolithic column and its application to purification of secondary alcohol dehydrogenase and alcohol oxidase.

PubMed

Isobe, Kimiyasu; Kawakami, Yoshimitsu

2007-03-09

A convection interaction media (trade name CIM, BIA Separation, Ljubljana, Slovenia) isobutyl monolithic disc was prepared by incubating a CIM epoxy monolithic disc with isobutylamine, and it was then applied to the purification of secondary alcohol dehydrogenase (S-ADH) and primary alcohol oxidase (P-AOD). Both enzymes were adsorbed on this column and eluted with high purity. Thus, S-ADH was purified to an electrophoretically homogeneous state by four column chromatographies using CIM DEAE-8 and CIM C4-8 tube monolithic columns, blue-Sepharose column and CIM isobutyl disc monolithic column. P-AOD was also purified to an electrophoretically homogeneous state by three column chromatographies of CIM DEAE-8 tube, CIM C4-8 tube and CIM isobutyl disc columns.

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.

Recent Progress in Monolithic Silica Columns for High-Speed and High-Selectivity Separations.

PubMed

Ikegami, Tohru; Tanaka, Nobuo

2016-06-12

Monolithic silica columns have greater (through-pore size)/(skeleton size) ratios than particulate columns and fixed support structures in a column for chemical modification, resulting in high-efficiency columns and stationary phases. This review looks at how the size range of monolithic silica columns has been expanded, how high-efficiency monolithic silica columns have been realized, and how various methods of silica surface functionalization, leading to selective stationary phases, have been developed on monolithic silica supports, and provides information on the current status of these columns. Also discussed are the practical aspects of monolithic silica columns, including how their versatility can be improved by the preparation of small-sized structural features (sub-micron) and columns (1 mm ID or smaller) and by optimizing reaction conditions for in situ chemical modification with various restrictions, with an emphasis on recent research results for both topics.

Evidence of linked biogeochemical and hydrological processes in homogeneous and layered vadose zone systems

NASA Astrophysics Data System (ADS)

McGuire, J. T.; Hansen, D. J.; Mohanty, B. P.

2010-12-01

Understanding chemical fate and transport in the vadose zone is critical to protect groundwater resources and preserve ecosystem health. However, prediction can be challenging due to the dynamic hydrologic and biogeochemical nature of the vadose zone. Additional controls on hydrobiogeochemical processes are added by subsurface structural heterogeneity. This study uses repacked soil column experiments to quantify linkages between microbial activity, geochemical cycling and hydrologic flow. Three “short” laboratory soil columns were constructed to evaluate the effects of soil layering: a homogenized medium-grained sand, homogenized organic-rich loam, and a sand-over-loam layered column. In addition, two “long” columns were constructed using either gamma-irradiated (sterilized) or untreated sediments to evaluate the effects of both soil layers and the presence of microorganisms. The long columns were packed identically; a medium-grained sand matrix with two vertically separated and horizontally offset lenses of organic-rich loam. In all 5 columns, downward and upward infiltration of water was evaluated to simulate rainfall and rising water table events respectively. In-situ colocated probes were used to measure soil water content, matric potential, Eh, major anions, ammonium, Fe2+, and total sulfide. Enhanced biogeochemical cycling was observed in the short layered column versus the short, homogeneous columns, and enumerations of iron and sulfate reducing bacteria were 1-2 orders of magnitude greater. In the long columns, microbial activity caused mineral bands and produced insoluble gases that impeded water flow through the pores of the sediment. Capillary barriers, formed around the lenses due to soil textural differences, retarded water flow rates through the lenses. This allowed reducing conditions to develop, evidenced by the production of Fe2+ and S2-. At the fringes of the lenses, Fe2+ oxidized to form Fe(III)-oxide bands that further retarded water flux. No such mineral bands developed in the sterilized column. As a consequence, water content in the lenses of the sterilized column was half that of the other column and flow rates through the lenses were an order of magnitude lower. This flow impedance limited the interaction and mixing of groundwater with infiltrating vadose zone water and led to the formation of geochemically distinct water masses residing in relatively close proximity to one another. Results provide a specific examples of the direct impact of biogeochemical cycling on water flow in the vadose zone and vice versa. In addition, these demonstrate that the presence of layers in vadose zone environments may be an important control on overall chemical fate and transport in subsurface systems.

Chemometrics applications in biotechnology processes: predicting column integrity and impurity clearance during reuse of chromatography resin.

PubMed

Rathore, Anurag S; Mittal, Shachi; Lute, Scott; Brorson, Kurt

2012-01-01

Separation media, in particular chromatography media, is typically one of the major contributors to the cost of goods for production of a biotechnology therapeutic. To be cost-effective, it is industry practice that media be reused over several cycles before being discarded. The traditional approach for estimating the number of cycles a particular media can be reused for involves performing laboratory scale experiments that monitor column performance and carryover. This dataset is then used to predict the number of cycles the media can be used at manufacturing scale (concurrent validation). Although, well accepted and widely practiced, there are challenges associated with extrapolating the laboratory scale data to manufacturing scale due to differences that may exist across scales. Factors that may be different include: level of impurities in the feed material, lot to lot variability in feedstock impurities, design of the column housing unit with respect to cleanability, and homogeneity of the column packing. In view of these challenges, there is a need for approaches that may be able to predict column underperformance at the manufacturing scale over the product lifecycle. In case such an underperformance is predicted, the operators can unpack and repack the chromatography column beforehand and thus avoid batch loss. Chemometrics offers one such solution. In this article, we present an application of chemometrics toward the analysis of a set of chromatography profiles with the intention of predicting the various events of column underperformance including the backpressure buildup and inefficient deoxyribonucleic acid clearance. Copyright © 2012 American Institute of Chemical Engineers (AIChE).

Off-Line Multidimensional Liquid Chromatography and Auto Sampling Result in Sample Loss in LC/LC–MS/MS

PubMed Central

2015-01-01

Large-scale proteomics often employs two orthogonal separation methods to fractionate complex peptide mixtures. Fractionation can involve ion exchange separation coupled to reversed-phase separation or, more recently, two reversed-phase separations performed at different pH values. When multidimensional separations are combined with tandem mass spectrometry for protein identification, the strategy is often referred to as multidimensional protein identification technology (MudPIT). MudPIT has been used in either an automated (online) or manual (offline) format. In this study, we evaluated the performance of different MudPIT strategies by both label-free and tandem mass tag (TMT) isobaric tagging. Our findings revealed that online MudPIT provided more peptide/protein identifications and higher sequence coverage than offline platforms. When employing an off-line fractionation method with direct loading of samples onto the column from an eppendorf tube via a high-pressure device, a 5.3% loss in protein identifications is observed. When off-line fractionated samples are loaded via an autosampler, a 44.5% loss in protein identifications is observed compared with direct loading of samples onto a triphasic capillary column. Moreover, peptide recovery was significantly lower after offline fractionation than in online fractionation. Signal-to-noise (S/N) ratio, however, was not significantly altered between experimental groups. It is likely that offline sample collection results in stochastic peptide loss due to noncovalent adsorption to solid surfaces. Therefore, the use of the offline approaches should be considered carefully when processing minute quantities of valuable samples. PMID:25040086

Research on miniature gas analysis systems

NASA Technical Reports Server (NTRS)

Angell, J. B.

1974-01-01

Technology for fabricating very small valves, whose function will be to introduce a small sample of the gas to be analyzed into the main carrier gas stream flowing through the chromatograph column is described. In addition, some analyses were made of the factors governing the resolution of gas chromatographs, particularly those with miniature columns. These analyses show how important the column lining thickness is in governing the ability of a miniature column to separate components of an unknown gas. A brief description of column lining factors is included. Preliminary work on a super small thermistor detector is included.