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Sample records for adsorption chromatographic xad

  1. RECOVERY OF MUTAGENICITY FROM DISINFECTED WATER BY XAD RESIN ADSORPTION COMPARED TO REVERSE OSMOSIS

    EPA Science Inventory

    Recovery of Mutagenicity from Disinfected Water Samples by XAD Resin Adsorption Compared to Reverse Osmosis

    K. M. Schenck1, T. F. Speth1, R. J. Miltner1, M. Sivaganesan1 and J. E. Simmons2

    1U.S. EPA, Office of Research and Development, NRMRL
    2U.S. EPA, Office of...

  2. CHEMICAL ANALYSIS OF REVERSE OSMOSIS MEMBRANE AND XAD RESIN ADSORPTION CONCENTRATES OF WATER DISINFECTED BY CHLORINATION OR OZONATION/CHLORINATION PROCESSES

    EPA Science Inventory


    Chemical Analysis of Reverse Osmosis Membrane and XAD Resin Adsorption Concentrates of Water Disinfected by Chlorination or Ozonation/Chlorination Processes.

    J. E. Simmons1, S.D. Richardson2, K.M. Schenck3, T. F. Speth3, R. J. Miltner3 and A. D. Thruston2

    1 NHEE...

  3. Synthesis and application of Amberlite xad-4 functionalized with alizarin red-s for preconcentration and adsorption of rhodium (III)

    PubMed Central

    2012-01-01

    A new chelating resin was prepared by coupling Amberlite XAD-4 with alizarin red-s through an azo spacer, characterized by infra-red spectroscopy and thermal analysis and studied for Rh(III) preconcentration using inductively coupled plasma atomic emission spectroscopy (ICP-AES) for rhodium monitoring in the environment. The optimum pH for sorption of the metal ion was 6.5. The sorption capacity was found 2.1 mg/g of resin for Rh(III). A recovery of 88% was obtained for the metal ion with 1.5 M HCl as eluting agent. Kinetic adsorption data were analyzed by adsorption and desorption times of Rh(III) on modified resin. Scat chard analysis revealed that the homogeneous binding sites were formed in the polymers. The linear regression equation was Q/C = –1.3169Q + 27.222 (R2 = 0.9239), for Rh were formed in the SPE sorbent,Kd and Qmax for the affinity binding sites were calculated to be 0.76 μmol/mL and 20.67 μmol/g, respectively. The equilibrium data and parameters of Rh(III) adsorption on modified resin were analyzed by Langmuir, Freundlich, Temkin and Redlich–Peterson models. The experimental adsorption isotherm was in good concordance with Langmuir and Freundlich models (R2 > 0.998) and based on the Langmuir isotherm the maximum amount of adsorption (qmax) was 4.842 mg/g. The method was applied for rhodium ions determination in environmental samples. with high recovery (>80%). PMID:23369526

  4. Adsorptive stripping voltammetric determination of imipramine, trimipramine and desipramine employing titanium dioxide nanoparticles and an Amberlite XAD-2 modified glassy carbon paste electrode.

    PubMed

    Sanghavi, Bankim J; Srivastava, Ashwini K

    2013-03-07

    An Amberlite XAD-2 (XAD2) and titanium dioxide nanoparticles (TNPs) modified glassy carbon paste electrode (XAD2-TNP-GCPE) was developed for the determination of imipramine (IMI), trimipramine (TRI) and desipramine (DES). The electrochemical behavior of these molecules was investigated employing cyclic voltammetry (CV), chronocoulometry (CC), electrochemical impedance spectroscopy (EIS) and adsorptive stripping differential pulse voltammetry (AdSDPV). After optimization of analytical conditions using a XAD2-TNP-GCPE electrode at pH 6.0 phosphate buffer (0.1 M), the peak currents were found to vary linearly with its concentration in the range of 1.30 × 10(-9) to 6.23 × 10(-6) M for IMI, 1.16 × 10(-9) to 6.87 × 10(-6) M for TRI and 1.43 × 10(-9) to 5.68 × 10(-6) M for DES. The detection limits (S/N = 3) of 3.93 × 10(-10), 3.51 × 10(-10) and 4.35 × 10(-10) M were obtained for IMI, TRI and DES respectively using AdSDPV. The prepared modified electrode showed several advantages such as a simple preparation method, high sensitivity, very low detection limits and excellent reproducibility. The proposed method was employed for the determination of IMI, TRI and DES in pharmaceutical formulations, blood serum and urine samples.

  5. Mutagenic activity in disinfected waters and recovery of the potent bacterial mutagen "MX" from water by XAD resin adsorption

    NASA Astrophysics Data System (ADS)

    Backlund, Peter; Wondergem, Erik; Kronberg, Leif

    Chlorination of humic water generated mutagenic activity in the Ames test. The formation of the potent bacterial mutagen 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX) and mutagenic activity were favoured by acidic chlorination conditions and high chlorine doses. Chlorinated humic waters from different locations differed slightly in the level of mutagenicity as well as in the proportion of activity derived from MX. Chlorination of an industrially polluted surface water with a low content of humic material generated an approximately equal level of mutagenicity (per mg of DOC) as that of chlorinated humic water, but only a minor part (26%) of the activity could be explained by the presence of MX. The mutagenicity and the amount of MX generated were substantially lower when using combined treatment methods (ClO2+Cl2, O3+Cl2) or when substituting chlorine by monochloramine or chlorine dioxide. The recovery of MX by XAD adsorption from water acidified to pH 2 was found to be quantitative.

  6. The Calculation of Adsorption Isotherms from Chromatographic Peak Shapes

    ERIC Educational Resources Information Center

    Neumann, M. G.

    1976-01-01

    Discusses the relationship between adsorption isotherms and elution peak shapes in gas chromatography, and describes a laboratory experiment which involves the adsorption of hexane, cyclohexane, and benzene on alumina at different temperatures. (MLH)

  7. New Method for Evaluating Irreversible Adsorption and Stationary Phase Bleed in Gas Chromatographic Capillary Columns

    SciTech Connect

    Wright, Bob W.; Wright, Cherylyn W.

    2012-10-26

    A novel method for the evaluation of gas chromatographic (GC) column inertness has been developed using a tandem GC approach. Typically column inertness is measured by analyte peak shape evaluation. In general, silica, glass, and metal surfaces are chemically reactive and can cause analyte adsorption, which typically is observed as chromatographic peak tailing. Adsorption processes produce broad, short chromatographic peaks that confound peak area determinations because a significant portion can reside in the noise. In addition, chromatographic surfaces and stationary phases can irreversibly adsorb certain analytes without obvious degradation of peak shape. The inertness measurements described in this work specifically determine the degree of irreversible adsorption behavior of specific target compounds at levels ranging from approximately 50 picograms to 1 nanogram on selected gas chromatographic columns. Chromatographic columns with 5% phenylmethylsiloxane, polyethylene glycol (wax), trifluoropropylsiloxane, and 78% cyanopropylsiloxane stationary phases were evaluated with a variety of phosphorus- and sulfur- containing compounds selected as test compounds due to their ease of adsorption and importance in trace analytical detection. In addition, the method was shown effective for characterizing column bleed.

  8. Chromatographic determination of the differential isosteric adsorption enthalpies and differential entropies on ordered silica materials.

    PubMed

    Grajek, H; Paciura-Zadrozna, J; Witkiewicz, Z

    2008-06-13

    The adsorption properties of the ordered mesoporous siliceous materials: MCM-41C16 (denoted as C16), MCM-41C16-SH and MCM-41C16-NH(2) (known as MCMs) having different surface functionalities were studied by inverse gas chromatography to assess their suitability for adsorption of analytes from gas and liquid phases. Polar and non-polar adsorbates were employed. The differential isosteric enthalpies, -DeltaH(ads), and differential entropies, -DeltaS(ads), of adsorption of different 'molecular probes' were determined chromatographically. A mathematical link between the -DeltaH(ads), and -DeltaS(ads) magnitudes and experimental data was derived through an Antoine-type equation. The present studies have been entirely restricted to the region of low adsorbate concentration. The problem of the interrelationship between the -DeltaH(ads), and -DeltaS(ads) values, known as the 'thermodynamic compensation effect', and interpretation of chromatographic data for the adsorption of different adsorbates on the MCMs have been considered in the light of both experimental data obtained in the present studies and the data available in the literature for siliceous adsorbents with randomly ordered structures. It was shown chromatographically that there is substantial parallelism between the magnitudes of the differential isosteric enthalpy and differential entropy for some 'molecular probes' chromatographed on C16 and its derivatives. Complementary information was obtained by atomic-force microscopy (AFM), X-ray photoelectron spectroscopy and X-ray diffraction (XRD) spectroscopy.

  9. Chromatographic and traditional albumin isotherms on cellulose: a model for wound protein adsorption on modified cotton.

    PubMed

    Edwards, J Vincent; Castro, Nathan J; Condon, Brian; Costable, Carmen; Goheen, Steven C

    2012-05-01

    Albumin is the most abundant protein found in healing wounds. Traditional and chromatographic protein isotherms of albumin binding on modified cotton fibers are useful in understanding albumin binding to cellulose wound dressings. An important consideration in the design of cellulosic wound dressings is adsorption and accumulation of proteins like albumin at the solid-liquid interface of the biological fluid and wound dressing fiber. To better understand the effect of fiber charge and molecular modifications in cellulose-containing fibers on the binding of serum albumin as observed in protease sequestrant dressings, albumin binding to modified cotton fibers was compared with traditional and chromatographic isotherms. Modified cotton including carboxymethylated, citrate-crosslinked, dialdehyde and phosphorylated cotton, which sequester elastase and collagenase, were compared for their albumin binding isotherms. Albumin isotherms on citrate-cellulose, cross-linked cotton demonstrated a two-fold increased binding affinity over untreated cotton. A comparison of albumin binding between traditional, solution isotherms and chromatographic isotherms on modified cellulose yielded similar equilibrium constants. Application of the binding affinity of albumin obtained in the in vitro protein isotherm to the in vivo wound dressing uptake of the protein is discussed. The chromatographic approach to assessment of albumin isotherms on modified cellulose offers a more rapid approach to evaluating protein binding on modified cellulose over traditional solution approaches.

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

    SciTech Connect

    Stanley, B.J.; Guiochon, G. Oak Ridge National Lab., TN )

    1994-11-01

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

  11. pH-dependence of single-protein adsorption and diffusion at a liquid chromatographic interface.

    PubMed

    Kisley, Lydia; Poongavanam, Mohan-Vivekanandan; Kourentzi, Katerina; Willson, Richard C; Landes, Christy F

    2016-02-01

    pH is a common mobile phase variable used to control protein separations due to the tunable nature of amino acid and adsorbent charge. Like other column variables such as column density and ligand loading density, pH is usually optimized empirically. Single-molecule spectroscopy extracts molecular-scale data to provide a framework for mechanistic optimization of pH. The adsorption and diffusion of a model globular protein, α-lactalbumin, was studied by single-molecule microscopy at a silica-aqueous interface analogous to aqueous normal phase and hydrophilic interaction chromatography and capillary electrophoresis interfaces at varied pH. Electrostatic repulsion resulting in free diffusion was observed at pH above the isoelectric point of the protein. In contrast, at low pH strong adsorption and surface diffusion with either no (D ∼ 0.01 μm(2) /s) or translational (D ∼ 0.3 μm(2) /s) motion was observed where the protein likely interacted with the surface through electrostatic, hydrophobic, and hydrogen bonding forces. The fraction of proteins immobilized could be increased by lowering the pH. These results show that retention of proteins at the silica interface cannot be viewed solely as an adsorption/desorption process and that the type of surface diffusion, which ultimately leads to ensemble chromatographic separations, can be controlled by tuning long-range electrostatic and short-range hydrophobic and hydrogen bonding forces with pH.

  12. Adsorption saturation and chromatographic distortion effects on passive headspace sampling with activated charcoal in fire debris analysis.

    PubMed

    Williams, Mary R; Fernandes, Denise; Bridge, Candice; Dorrien, Derek; Elliott, Stefanie; Sigman, Michael

    2005-03-01

    Distortion of the chromatographic profile obtained for hydrocarbons that have been sampled by adsorption onto activated charcoal is a well-known phenomenon. The work reported here helps to better define the causes of chromatographic profile distortion and offers a potential method to avoid chromatographic distortion in some cases through a subsampling technique. The recovery of hydrocarbons from an equimolar mixture was investigated to determine the influence of hydrocarbon concentration on the molar ratios of recovered components. In a one-quart container, hydrocarbon volumes as small as 24 microL (liquid) were sufficient to saturate the surface area available for adsorption on a 99.0 mm2 square of activated charcoal, resulting in significant distortions in the molar ratio and the chromatographic profile of the recovered hydrocarbons. Passive headspace sampling of a similarly small volume of unweathered gasoline spiked onto carpet padding resulted in a significant distortion of the chromatographic profile. The chromatographic profile of the recovered hydrocarbons closely resembled 75% weathered gasoline. Heating the container spiked with unweathered gasoline to evenly distribute the components and then removing a subsample of the carpet padding to a second container for passive headspace analysis greatly reduced the amount of distortion in the resulting chromatogram.

  13. Time-resolved chromatographic analysis and mechanisms in adsorption and catalysis.

    PubMed

    Roubani-Kalantzopoulou, Fani

    2009-03-06

    The main object of this review is the study of fundamentals of adsorption and heterogeneous catalysis, a benefit for the understanding of adsorptive and catalytic properties. This work aims to define and record, with the utmost accuracy, the phenomena and the possible reactions. A new methodology for the study of the adsorption is presented, which is a version of the well-known inverse gas chromatography. This reversed-flow inverse gas chromatography (RF-IGC) is technically very simple, and it is combined with a mathematical analysis that gives the possibility for the estimation of various physicochemical parameters related to adsorbent or catalyst characterization, under conditions compatible with the operation of real adsorbents and catalysts. On this base, this methodology has been successfully applied to the study of the impact of air pollutants, volatile organic and/or inorganic, on many solids such as marbles, ceramics, oxide-pigments of works of art, building materials, authentic statues of the Greek Archaeological Museums. Moreover, this methodology proved to be a powerful tool for studying the topography of active sites of heterogeneous surfaces in the nano-scale domain. Thus, some very important local quantities for the surface chemistry have been determined experimentally for many solids including thin films. These physicochemical local quantities (among which adsorption energy and entropy, surface diffusion coefficient, probability density function) have been determined from the experimental pairs of height of extra chromatographic peaks and time by a nonlinear least-squares method, through personal computer programs written in GW BASIC and lately in FORTRAN. Through the time-resolved analysis the surface characterization of the examined materials took place. In addition, the kinetic constants responsible for adsorption/desorption and surface chemical reactions have also been calculated. Thus, important answers have been provided to the following

  14. Studies on the batch adsorption of plasmid DNA onto anion-exchange chromatographic supports.

    PubMed

    Ferreira, G N; Cabral, J M; Prazeres, D M

    2000-01-01

    The adsorption of a supercoiled 4.8 kbp plasmid onto quaternary ammonium anion-exchangers was studied in a finite bath. Equilibrium experiments were performed with pure plasmid, at 25 degrees C, using commercial Q-Sepharose matrices differing in particle diameter (High Performance, 34 microm; Fast Flow, 90 microm; and Big Beads, 200 microm) and a recently commercialized ion-exchanger, Streamline QXL (d(p) = 200 microm) at different salt concentrations (0.5, 0.7, and 1 M NaCl). Plasmid adsorption was found to follow second-order kinetics (Langmuir isotherm) with average association constants K(A) = 0.32+/-0.12 mL microg(-)(1) and K(A) = 0.25+/-0.15 mL microg(-1) at 0.5 and 0.7 M Nacl, respectively. The maximum binding capacities were not dependent on the ionic strength in the range 0.5-0.7 M but decreased with increasing particle diameter, suggesting that adsorption mainly occurs at the surface of the particles. No adsorption was found at 1 M NaCl. A nonporous model was applied to describe the uptake rate of plasmid onto Streamline QXL at 0.5 M NaCl. The overall process rate was controlled by mass transfer in the regions of low relative amounts of adsorbent (initial stages) and kinetically controlled in the later stages of the process for high relative amounts of adsorbent. The forward reaction rate constant (k(1) = 0.09+/-0.01 mL mg(-1) s(-1)) and film mass transfer coefficient (K(f) = (6 +/- 2) x 10(-4) cm s(-1)) were calculated. Simulations were performed to study the effect of the relative amount of adsorbent on the overall process rate, yield, and media capacity utilization.

  15. Isolation of organic acids from large volumes of water by adsorption chromatography

    USGS Publications Warehouse

    Aiken, George R.

    1984-01-01

    The concentrations of dissolved organic carbon from most natural waters ranges from 1 to 20 milligrams carbon per liter, of which approximately 75 percent are organic acids. These acids can be chromatographically fractionated into hydrophobic organic acids, such as humic substances, and hydrophilic organic acids. To effectively study any of these organic acids, they must be isolated from other organic and inorganic species, and concentrated. Usually, large volumes of water must be processed to obtain sufficient quantities of material, and adsorption chromatography on synthetic, macroporous resins has proven to be a particularly effective method for this purpose. The use of the nonionic Amberlite XAD-8 and Amberlite XAD-4 resins and the anion exchange resin Duolite A-7 for isolating and concentrating organic acids from water is presented.

  16. Calibration of polydimethylsiloxane and XAD-Pocket passive air samplers (PAS) for measuring gas- and particle-phase SVOCs

    NASA Astrophysics Data System (ADS)

    Okeme, Joseph O.; Saini, Amandeep; Yang, Congqiao; Zhu, Jiping; Smedes, Foppe; Klánová, Jana; Diamond, Miriam L.

    2016-10-01

    Polydimethylsiloxane (PDMS) has seen wide use as the stationary phase of gas chromatographic columns, a passive sampler in water, and recently as a personal exposure sampler, while styrene divinyl-benzene copolymer (XAD) has been used extensively as a passive air sampler outdoors and indoors. We have introduced PDMS and XAD-Pocket as new indoor passive air samplers (PASs). The XAD-Pocket was designed to maximize the surface area-to-volume ratio of XAD and to minimize obstruction of air flow by the sampler housing. Methods were developed to expedite the use of these PASs for measuring phthalates, novel brominated flame-retardants (NFRs) and polybrominated diphenyl ethers (PBDEs) indoors. Sampling rates, Rs, (m3 day-1), were measured during a 7-week calibration study. Variability within and between analyte groups was not statistically significant. As a result, generic values of 0.8 ± 0.4 and 0.5 ± 0.3 m3 day-1 dm-2 are recommended for PDMS and XAD-Pocket for a 50-day deployment time, respectively. PDMS has a higher uptake rate and is easier to use than XAD-Pocket.

  17. Comparative study of the dynamic gravimetric and pulse chromatographic methods for the determination of Henry constants of adsorption for VOC zeolite systems

    NASA Astrophysics Data System (ADS)

    Nokerman, J.; Canet, X.; Mougin, P.; Limborg-Noetinger, S.; Frère, M.

    2005-09-01

    In this paper, we propose a comparative study between a gravimetric apparatus operating under dynamic conditions and a pulse chromatographic device developed for the determination of Henry constants of adsorption for VOC-zeolite systems. In both cases, we provide a description of the experimental set-up and procedure, as well as a complete report on the treatment of the rough experimental data. The experimental errors are also discussed. The comparison work is based on the study of the adsorption of toluene on a NaY zeolite (Si/Al 2.43) for temperatures ranging from 503 to 623 K. The maximal discrepancy found between the experimental Henry constants was 15.0%. The pulse chromatographic method is only dedicated to high-temperature measurements. For low-temperature experiments, the rough data cannot be treated in an efficient way, and it is not possible to obtain reliable Henry constant values. The dynamic gravimetric method is not temperature limited. It is however time-consuming, especially when low-temperature measurements (not presented in this paper) are concerned. Both methods are complementary if the determination of Henry constants is required in a wide temperature range.

  18. Comparison of humic substances isolated from peatbog water by sorption on DEAE-cellulose and amberlite XAD-2

    USGS Publications Warehouse

    Hejzlar, J.; Szpakowska, B.; Wershaw, R. L.

    1994-01-01

    Aquatic humic substances (AHS) were isolated from peatbog water by adsorption (1) on diethylaminoethyl cellulose (DEAE-C) and (2) on Amberlite XAD-2 (XAD) to compare yields of the methods and the composition of the isolated AHS. To provide a detailed comparison, the isolates were fractionated using size-exclusion and hydrophobic-interaction chromatography on Sephadex G-50. The fractions were characterized by ultraviolet-visible, infrared and 13C-nuclear magnetic spectroscopies and analyzed for elemental, functional-group, carbohydrate and amino acid compositions. More AHS adsorbed onto DEAE-C than onto XAD-2 (94 and 74%, respectively). However, only 76% of the AHS adsorbed onto DEAE-C was recovered using 0.1 M NaOH, whereas 98% of the AHS adsorbed onto XAD was released by consecutive elution with 1 M NH4OH (91%) and methanol (7%). Four main fractions of different composition were obtained from each of the alkali-desorbed AHS samples by Sephadex-gel chromatography. General agreement was found in relative amounts, spectroscopic characteristics and composition of corresponding fractions of both isolates except nitrogen content, which was significantly higher in AHS isolated with XAD, apparently due to the reaction of AHS with NH4OH used for the desorption from the resin.Aquatic humic substances (AHS) were isolated from peatbog water by adsorption (1) on diethylaminoethyl cellulose (DEAE-C) and (2) on Amberlite XAD-2 (XAD) to compare yields of the methods and the composition of the isolated AHS. To provide a detailed comparison, the isolates were fractionated using size-exclusion and hydrophobic-interaction chromatography on Sephadex G-50. The fractions were characterized by ultraviolet-visible, infrared and 13C-nuclear magnetic spectroscopies and analyzed for elemental, functional-group, carbohydrate and amino acid compositions. More AHS adsorbed onto DEAE-C than onto XAD-2 (94 and 74%, respectively). However, only 76% of the AHS adsorbed onto DEAE-C was recovered

  19. Quantitative evaluation of XAD-8 and XAD-4 resins used in tandem for removing organic solutes from water

    USGS Publications Warehouse

    Malcolm, R.L.; MacCarthy, P.

    1992-01-01

    The combined XAD-8 and XAD-4 resin procedure for the isolation of dissolved organic solutes from water was found to isolate 85% or more of the organic solutes from Lake Skjervatjern in Norway. Approximately 65% of the dissolved organic carbon (DOC) was first removed on XAD-8 resin, and then an additional 20% of the DOC was removed on XAD-4 resin. Approximately 15% of the DOC solutes (primarily hydrophilic neutrals) were not sorbed or concentrated by the procedure. Of the 65% of the solutes removed on XAD-8 resin, 40% were fulvic acids, 16% were humic acids, and 9% were hydrophobic neutrals. Approximately 20% of the hydrophilic solutes that pass through the XAD-8 resin were sorbed solutes on the second resin, XAD-4 (i.e., they were hydrophobic relative to the XAD-4 resin). The fraction sorbed on XAD-4 resin was called XAD-4 acids because it represented approximately 85-90% of the hydrophilic XAD-8 acid fraction according to the original XAD-8 fractionation procedure. The recovery of hydrophobic acids (fulvic acids and humic acids) and the hydrophobic neutral fraction from XAD-8 resin was essentially quantitative at 96%, 98%, and 86%, respectively. The recovery of XAD-4 acids from the XAD-4 resin was only about 50%. The exact reason for this moderately low recovery is unknown, but could result from ??-?? bonding between these organic solutes and the aromatic matrix of XAD-4. The hydrophobic/hydrophilic solute separation on XAD-8 resin for water from background Side A and Side B of the lake was almost identical at 65 and 67%, respectively. This result suggested that both sides of the lake are similar in organic chemical composition even though the DOC variation from side to side is 20%.

  20. Prediction of the sorption capacities and affinities of organic chemicals by XAD-7.

    PubMed

    Yang, Kun; Qi, Long; Wei, Wei; Wu, Wenhao; Lin, Daohui

    2016-01-01

    Macro-porous resins are widely used as adsorbents for the treatment of organic contaminants in wastewater and for the pre-concentration of organic solutes from water. However, the sorption mechanisms for organic contaminants on such adsorbents have not been systematically investigated so far. Therefore, in this study, the sorption capacities and affinities of 24 organic chemicals by XAD-7 were investigated and the experimentally obtained sorption isotherms were fitted to the Dubinin-Ashtakhov model. Linear positive correlations were observed between the sorption capacities and the solubilities (SW) of the chemicals in water or octanol and between the sorption affinities and the solvatochromic parameters of the chemicals, indicating that the sorption of various organic compounds by XAD-7 occurred by non-linear partitioning into XAD-7, rather than by adsorption on XAD-7 surfaces. Both specific interactions (i.e., hydrogen-bonding interactions) as well as nonspecific interactions were considered to be responsible for the non-linear partitioning. The correlation equations obtained in this study allow the prediction of non-linear partitioning using well-known chemical parameters, namely SW, octanol-water partition coefficients (KOW), and the hydrogen-bonding donor parameter (αm). The effect of pH on the sorption of ionizable organic compounds (IOCs) could also be predicted by combining the correlation equations with additional equations developed from the estimation of IOC dissociation rates. The prediction equations developed in this study and the proposed non-linear partition mechanism shed new light on the selective removal and pre-concentration of organic solutes from water and on the regeneration of exhausted XAD-7 using solvent extraction.

  1. Adsorption of pesticides on resins.

    PubMed

    Kyriakopoulos, Grigorios; Hourdakis, Adamadia; Doulia, Danae

    2003-03-01

    The objective of this work was to assess the capability of organic hydrophobic polymeric resins Amberlite XAD-4 and XAD-7 to remove the pesticides alachlor and amitrole from water. The pesticides adsorption on the two different adsorbents was measured by batch equilibrium technique and isotherm types and parameters were estimated. Two theoretical models were applied based on a Freundlich and a Langmuir isotherms. The effect of pesticides chemical composition and structure as well as the nature of solid surface on the efficiency of adsorption was evaluated. The influence of pH also was studied. In low pH solutions adsorption of amitrole was higher upon the nonionic aliphatic acrylic ester copolymer XAD-7 in comparison to the nonionic, crosslinked macroreticular copolymer of styrene divinylbenzene XAD-4. In neutral and intermediate pH solutions the polar acrylic ester copolymer XAD-7 was more effective to the retention of alachlor. The acrylic ester copolymer showed at pH 3 the lower effectiveness in alachlor removal from water. The data of the adsorption isotherms of pesticides upon the examined polymeric resins seemed to conform to both the Freundlich and the Langmuir isotherm models.

  2. Comparison of XAD macroporous resins for the concentration of fulvic acid from aqueous solution

    USGS Publications Warehouse

    Aiken, G.R.

    1979-01-01

    Five macroreticular, nonlonlc AmberlHe XAD resins were evaluated for concentration and Isolation of fulvlc acid from aqueous solution. The capacity of each resin for fulvlc acid was measured by both batch and column techniques. Elution efficiencies were determined by desorptlon with 0.1 N NaOH. Highest recoveries were obtained with the acrylic ester resins which proved to be most efficient for both adsorption and elution of fulvlc acid. Compared to the acrylic ester resins, usefulness of the styrene dvlnybenzene resins to remove fulvlc acid is limited because of slow diffusion-controlled adsorption and formation of charge-transfer complexes, which hinders elution. ?? 1979 American Chemical Society.

  3. Sodium citrate and potassium phosphate as alternative adsorption buffers in hydrophobic and aromatic thiophilic chromatographic purification of plasmid DNA from neutralized lysate.

    PubMed

    Bonturi, Nemailla; Radke, Vanessa Soraia Cortez Oliveira; Bueno, Sônia Maria Alves; Freitas, Sindélia; Azzoni, Adriano Rodrigues; Miranda, Everson Alves

    2013-03-01

    The number of studies on gene therapy using plasmid vectors (pDNA) has increased in recent years. As a result, the demand for preparations of pDNA in compliance with recommendations of regulatory agencies (EMEA, FDA) has also increased. Plasmid DNA is often obtained through fermentation of transformed Escherichia coli and purification by a series of unit operations, including chromatography. Hydrophobic interaction chromatography (HIC) and thiophilic aromatic chromatography (TAC), both using ammonium sulfate buffers, are commonly employed with success. This work was aimed at studying the feasibility of utilizing alternative salts in the purification of pDNA from neutralized lysate with phenyl-agarose (HIC) and mercaptopyrimidine-agarose (TAC) adsorbents. Their selectivity toward sc pDNA was evaluated through adsorption studies using 1.5 mol/L sodium citrate and 2.0 mol/L potassium phosphate as adsorption buffers. Chromatography with mercaptopyrimidine-agarose adsorbent and 1.5 mol/L sodium citrate was able to recover 91.1% of the pDNA with over 99.0% removal of gDNA and endotoxin. This represents a potential alternative for the primary recovery of sc pDNA. However, the most promising result was obtained using 2.0 mol/L potassium phosphate buffer and a mercaptopyrimidine-agarose column. In a single chromatographic step, this latter buffer/adsorbent system recovered 68.5% of the pDNA with 98.8% purity in accordance with the recommendations of regulatory agencies with regard to RNA and endotoxin impurity.

  4. Energy-efficient recovery of butanol from model solutions and fermentation broth by adsorption.

    PubMed

    Qureshi, N; Hughes, S; Maddox, I S; Cotta, M A

    2005-07-01

    This article discusses the separation of butanol from aqueous solutions and/or fermentation broth by adsorption. Butanol fermentation is also known as acetone butanol ethanol (ABE) or solvent fermentation. Adsorbents such as silicalite, resins (XAD-2, XAD-4, XAD-7, XAD-8, XAD-16), bone charcoal, activated charcoal, bonopore, and polyvinylpyridine have been studied. Use of silicalite appears to be the more attractive as it can be used to concentrate butanol from dilute solutions (5 to 790-810 g L(-1)) and results in complete desorption of butanol (or ABE). In addition, silicalite can be regenerated by heat treatment. The energy requirement for butanol recovery by adsorption-desorption processes has been calculated to be 1,948 kcal kg(-1) butanol as compared to 5,789 kcal kg(-1) butanol by steam stripping distillation. Other techniques such as gas stripping and pervaporation require 5,220 and 3,295 kcal kg(-1) butanol, respectively.

  5. Comparison of two polarity measurements of hydrophobic organic matter for the evaluation of water treatment processes: XAD resin and PRAM.

    PubMed

    Philibert, Marc; Rosario-Ortiz, Fernando; Suffet, Mel

    2012-01-01

    Dissolved organic matter (DOM) is a mixture of thousands of organic molecules wide-ranging in molecular weight, polarity and physicochemical properties. DOM is responsible for multiple water treatment issues such as trihalomethane (THM) formation potential and membrane fouling. Two methods of evaluating the polarity of DOM are being used for water treatment application: a serial XAD resin adsorption method at acid pH and the polarity rapid assessment method (PRAM) by parallel solid phase extraction (SPE) cartridges at natural pH. These two methods have been described by their authors as able to define a hydrophobic fraction though they do so by sorption onto different types of material at different pHs. The first part of this study compared the PRAM and XAD methods and showed that the hydrophobic fractions defined by the two approaches were not correlated. This result highlighted the difficulties in defining fractions as 'hydrophobic material'. It appeared that the sorbents for XAD-8 (an acrylic polymer containing oxygen) at pH <3 and C-18 (a pure hydrocarbon polymer coating on silica particles) at neutral or pH <3 did not retain similar hydrophobic fractions. This hypothesis was verified by fluorescence spectroscopy of the effluent of the XAD-8 resin and PRAM C-18 SPE cartridge. Finally the study concentrated on the use of fluorescence and ultrafiltration methods in series with PRAM to gain more insight into the structure and characteristics of the hydrophobic DOM present in drinking water sources. This evaluation showed that the smaller molecular weight fraction of DOM (<1 kDa) had a higher percentage of hydrophobic character and that the fluorescence-defined aromatic protein fraction was the most hydrophilic.

  6. Themodynamics of adsorption and patterns of the gas-chromatographic retention of cyclic amines on surfaces of graphitized thermal carbon black

    NASA Astrophysics Data System (ADS)

    Yashkina, E. A.; Yashkin, S. N.; Svetlov, D. A.; Gorshkov, V. V.

    2015-09-01

    The thermodynamic characteristics of adsorption (TCA) of aniline, cyclohexylamine, and some of their derivatives on surfaces of graphitized thermal carbon black (GTC) are experimentally determined under conditions of gas-adsorption chromatography. It is concluded that the TCA values for the studied compounds depend to a large extent on the features of the geometrical and electronic structure of molecules in the gas phase. The effect of the sp 3- sp 2-rehybridization of nitrogen atoms upon moving from molecules of unsubstituted aniline to N-methyl- and N,N-dimethylanilines are determined, along with the ortho-effects in 2-methyland 2,6-dimethylanilines on the TCA values. It is shown that the above intramolecular effects result in nonadditive contributions to the energy of adsorption of the NH2-group in the a number of the studied compounds. Values of the thermal component of adsorption entropy are calculated, allowing conclusions on the physical state of the molecules of the studied compounds in the field of GTC adsorption forces. The mobility of adsorbate molecules is estimated using models of delocalized and localized adsorption. It is shown that in the series of ortho- meta- para-substituted anilines, the para-isomer is characterized by the highest values of retention on GTC, while the relative order of ortho- and meta-isomer elution is determined by the Van der Waals sizes of substituents in aromatic rings. A conclusion is reached on the high structural selectivity of a GTC surface in respect to positional isomers in the series of studied aniline derivatives.

  7. Selective adsorption of flavor-active components on hydrophobic resins.

    PubMed

    Saffarionpour, Shima; Sevillano, David Mendez; Van der Wielen, Luuk A M; Noordman, T Reinoud; Brouwer, Eric; Ottens, Marcel

    2016-12-09

    This work aims to propose an optimum resin that can be used in industrial adsorption process for tuning flavor-active components or removal of ethanol for producing an alcohol-free beer. A procedure is reported for selective adsorption of volatile aroma components from water/ethanol mixtures on synthetic hydrophobic resins. High throughput 96-well microtiter-plates batch uptake experimentation is applied for screening resins for adsorption of esters (i.e. isoamyl acetate, and ethyl acetate), higher alcohols (i.e. isoamyl alcohol and isobutyl alcohol), a diketone (diacetyl) and ethanol. The miniaturized batch uptake method is adapted for adsorption of volatile components, and validated with column breakthrough analysis. The results of single-component adsorption tests on Sepabeads SP20-SS are expressed in single-component Langmuir, Freundlich, and Sips isotherm models and multi-component versions of Langmuir and Sips models are applied for expressing multi-component adsorption results obtained on several tested resins. The adsorption parameters are regressed and the selectivity over ethanol is calculated for each tested component and tested resin. Resin scores for four different scenarios of selective adsorption of esters, higher alcohols, diacetyl, and ethanol are obtained. The optimal resin for adsorption of esters is Sepabeads SP20-SS with resin score of 87% and for selective removal of higher alcohols, XAD16N, and XAD4 from Amberlite resin series are proposed with scores of 80 and 74% respectively. For adsorption of diacetyl, XAD16N and XAD4 resins with score of 86% are the optimum choice and Sepabeads SP2MGS and XAD761 resins showed the highest affinity towards ethanol.

  8. Direct observation of intraparticle equilibration and the rate-limiting step in adsorption of proteins in chromatographic adsorbents with confocal laser scanning microscopy.

    PubMed

    Kasche, Volker; de Boer, Michael; Lazo, Cesar; Gad, Moustafa

    2003-06-25

    The adsorption of different proteins in a single biospecific and hydrophobic adsorbent particle for preparative protein chromatography has been observed directly by confocal laser scanning microscopy as a function of time at a constant bulk concentration c(b). The bulk concentration was in the non-linear part of the adsorption isotherm. At all times the concentration of free protein at the particle surface was almost equal to the bulk content indicating that external mass transfer resistance is not rate limiting for the adsorption under these conditions. Inside the particles a distinct maximum in adsorbed and free protein concentration that moved inside to a distance of approximately 0.2 R (R particle radius) from the particle surface, was observed. This is due to a decreasing solid-phase density and adsorptive capacity in the particle between 0.8 R and R indicating that the fraction of macropores (or void space) is larger in the outer than in the inner part of the adsorbent particles. By increasing the bulk concentration by a factor of 10 the equilibration time was reduced by about the same magnitude. This is in agreement with the concentration dependence of the effective pore diffusion coefficient D(p,eff)=D(p)/[epsilon(p)[1+nK/(K +c)(2)

  9. Adsorption and desorption characteristics of adlay bran free phenolics on macroporous resins.

    PubMed

    Yang, Qingyun; Zhao, Mouming; Lin, Lianzhu

    2016-03-01

    In this study, the adsorption and desorption characteristics of six macroporous resins including XAD-7HP, XAD-16, HP-20, HP-2MGL, SP-207 and SP-825 for enrichment of adlay bran free phenolics were studied. XAD-16, SP-207 and SP-825 were chosen for further study due to their strong adsorption and desorption capacities. XAD-16, SP-207 and SP-825 had similar phenolics adsorption/desorption behaviors. Pseudo-second-order kinetics model and Freundlich isotherm model were suitable for describing the whole exothermic and physical adsorption processes of adlay bran free phenolics on XAD-16, SP-207 and SP-825. After treatment with gradient elution on XAD-16 resin column, the free phenolics were mostly enriched (from 89.61 to 1015.26mg/100g) in 50% ethanol fraction. The oxygen radical absorbance capacity of 50% ethanol fraction was eight times higher than that of the crude extract. Therefore, the production of highly concentrated phenolics might expand the application of adlay bran used as a bioactive ingredient in functional food.

  10. Unfolding and aggregation of a glycosylated monoclonal antibody on a cation exchange column. Part I. Chromatographic elution and batch adsorption behavior.

    PubMed

    Guo, Jing; Zhang, Shaojie; Carta, Giorgio

    2014-08-22

    A glycosylated IgG2 monoclonal antibody exhibits a two-peak elution behavior when loaded on a strong cation exchange column and eluted with either a linear salt gradient or two salt steps at increasing salt concentrations. The two-peak behavior is more pronounced for conditions where the initial antibody binding is stronger, i.e. at lower pH and buffer concentration, where the hold time prior to elution is longer, where the protein mass load is lower, and where the load flow rate is higher. The effect is also dependent on the resin type, being prominent for the polymer-functionalized resin Fractogel EMD SO₃(-) and virtually absent for a macroporous resin with similar backbone but no grafted polymers. Size exclusion chromatography and dynamic light scattering show that the early eluting peak consists exclusively of the native monomeric species while the late eluting peak is a mixture of monomeric and aggregated species. Batch adsorption/desorption experiments show that the bound protein can be desorbed in two steps, with a fraction desorbed in 0.33 M NaCl, corresponding to native monomer, and a second fraction desorbed in 1M NaCl. The latter fraction decreases with protein mass load and becomes almost negligible when the resin is initially completely saturated with protein. Confocal laser scanning microscopy showed that the two-peak elution/desorption behavior is related to the unique kinetics of protein binding in the Fractogel resin. Following partial loading of the resin, the bound protein migrates toward the center of the particles during a hold step and is redistributed across the particle volume attaining low local bound protein concentrations. For these conditions the protein is apparently destabilized forming a strongly-bound unfolded intermediate that, in turn, generates aggregates upon elution in high salt.

  11. Purification of siderophores of Alcaligenes faecalis on Amberlite XAD.

    PubMed

    Sayyed, R Z; Chincholkar, S B

    2006-05-01

    Studies on siderophore production using Alcaligenes faecalis BCCM ID 2374 revealed hydroxamate and catecholate type of siderophores at 347 microg mL-1. These fractions were purified on Amberlite XAD-4 column, which resulted in the separation of two bands having absorption maxima at 264 and 224 nm. The amount of pure siderophore obtained in powdered form from first and second fraction was 297 and 50 microg mL-1 respectively.

  12. Adsorption properties of macroporous adsorbent resins for separation of anthocyanins from mulberry.

    PubMed

    Chen, Yao; Zhang, Weijie; Zhao, Ting; Li, Fang; Zhang, Min; Li, Jing; Zou, Ye; Wang, Wei; Cobbina, Samuel J; Wu, Xiangyang; Yang, Liuqing

    2016-03-01

    In this study, the adsorption/desorption characteristics of mulberry anthocyanins (MA) on five types of macroporous resins (XAD-7HP, AB-8, HP-20, D-101 and X-5) were evaluated, XAD-7HP and AB-8 showed higher adsorption/desorption capacities. On the basis of static adsorption test, XAD-7HP and AB-8 resins were selected for kinetics, isotherms and thermodynamics. The adsorption mechanism indicated that the process was better explained by pseudo-first-order kinetics and the Langmuir isotherm model, and the thermodynamics tests showed that the processes were exothermic, spontaneous and thermodynamically feasible. Dynamic tests were performed on a column packed with XAD-7HP and AB-8, and breakthrough volume was reached at 15 and 14 bed volumes of MA solution, respectively. The purity of the fraction by 40% ethanol elution on XAD-7HP reached 93.6%, from which cyanidin-3-glucoside and cyanidin-3-rutinoside were identified by HPLC-ESI-MS/MS. The method could be used to prepare high purity anthocyanins from mulberry fruits as well as other plants.

  13. Adsorption characteristics and preparative separation of chaetominine from Aspergillus fumigatus mycelia by macroporous resin.

    PubMed

    Liu, Changqing; Jiao, Ruihua; Yao, Lingyun; Zhang, Yupeng; Lu, Yanhua; Tan, Renxiang

    2016-03-15

    Chaetominine (CHA) is a quinazolinone alkaloid with strong anti-cancer activity produced by Aspergillus fumigatus CY018. For recovering CHA from A. fumigates efficiently, adsorption and desorption capacities of eight macroporous resins were tested in this work. Based on batch experiments, XAD-16 resin was revealed the best adsorption and desorption performance among all the tested resins. Then, adsorption kinetics and adsorption isotherms were constructed on XAD-16 resin, and the experimental data were fitted well to the pseudo first-order kinetics and Freundlick isotherm model. In the dynamic adsorption and desorption, the purity of CHA increased from 0.0314% (w/w) in the crude extract to 57.86% in the final product with recovery yield of 70.56% by a one-step treatment. Moreover, the experiments were also performed in a lab scale-up scale, in which the purity and recovery of CHA were 56.12% (w/w) and 68.02%, respectively. In addition, XAD-16 resin could be recycled 3 times for CHA separation after regeneration without adverse effects on adsorption/desorption performance. These results suggested that XAD-16 resin adsorption could act as a useful and economic method for recovering CHA from A. fumigatus.

  14. Comparison of extracts and toxicities of organic compounds in drinking water concentrated by single and composite XAD resins.

    PubMed

    Zhou, Xue; Xiang, Lunhui; Wu, Fenghong; Peng, Xiaoling; Xie, Hong; Wang, Jiachun; Yang, Kedi; Lu, Wenqing; Wu, Zhigang

    2013-12-01

    We compared extracts and toxicities of organic compounds (OCs) in drinking water concentrated by composite XAD-2/8 resin (mixed with an equal volume of XAD-2 and XAD-8 resins) with those extracted by single XAD-2 (non-polar) and XAD-8 (polar) resins. Drinking water was processed from raw water of the Han River and the Yangtze River in Wuhan section, China. The extraction efficiency of all resins was controlled at 30%. The types of extracted OCs were detected by gas chromatography-mass spectrometry, and the cytotoxicity and genotoxicity were assessed by MTT (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) and comet assays, respectively, in human hepatoma HepG2 cells. Our results showed that XAD-2/8 extracted a larger variety of OCs, compared with XAD-8 and XAD-2. The cytotoxicity and genotoxicity of extracted OCs were in the order of XAD-8> XAD-2/8> XAD-2 at almost all tested concentrations after 24 h treatment (P < 0.05). Our findings suggest that single XAD resin selectively extracts either polar or non-polar OCs, which would lead to over- or under-estimation of the toxicity of drinking water. Nevertheless, composite resin extracts both polar and non-polar OCs, and could be utilized as a useful extraction technique to evaluate the level and toxicity of OCs in drinking water.

  15. Absorption and desorption behaviour of the flavonoids from Glycyrrhiza glabra L. leaf on macroporous adsorption resins.

    PubMed

    Dong, Yi; Zhao, Mouming; Sun-Waterhouse, Dongxiao; Zhuang, Mingzhu; Chen, Huiping; Feng, Mengying; Lin, Lianzhu

    2015-02-01

    The kinetics of adsorption and desorption behaviours of five macroporous resins for enriching flavonoids from Glycyrrhizaglabra L. leaf were investigated. All five resins showed similar and effective adsorption and desorption properties. A pseudo-second-order kinetics model was suitable for evaluating the whole adsorption process. Additionally, two representative resins (XAD-16 and SP825) were chosen for adsorption thermodynamics study. The adsorption of the representative resins was an exothermic and physical adsorption process. Further column chromatography of XAD-16 and SP825 showed that the total flavonoids (from 16.8% to 55.6% by XAD-16 and to 53.9% by SP825) and pinocembrin (from 5.49% to 15.2% by XAD-16 and to 19.8% by SP825) were enriched in 90% ethanol fractions. Meanwhile, the antioxidant capacities and nitrite-scavenging capacities were 2-3times higher than those of the crude extract. The fractions with high flavonoid and pinocembrin contents could be used as biologically active ingredients in functional food.

  16. 2, 4 dichlorophenol (2, 4-DCP) sorption from aqueous solution using granular activated carbon and polymeric adsorbents and studies on effect of temperature on activated carbon adsorption.

    PubMed

    Ghatbandhe, A S; Yenkie, M K N

    2008-04-01

    Adsorption equilibrium, kinetics and thermodynamics of 2,4-dichlorophenol (2,4-DCP), one of the most commonly used chlorophenol, onto bituminous coal based Filtrasorb-400 grade granular activated carbon, were studied in aqueous solution in a batch system with respect to temperature. Uptake capacity of activated carbon found to increase with temperature. Langmuir isotherm models were applied to experimental equilibrium data of 2, 4-DCP adsorption and competitive studies with respect to XAD resin were carried out. Equilibrium data fitted very well to the Langmuir equilibrium model. Adsorbent monolayer capacity 'Q0, Langmuir constant 'b' and adsorption rate constant 'k(a)' were evaluated at different temperatures for activated carbon adsorption. This data was then used to calculate the energy of activation of adsorption and also the thermodynamic parameters, namely the free energy of adsorption, deltaG0, enthalpy of adsorption, deltaH0 and the entropy of adsorption deltaS0. The obtained results showed that the monolayer capacity increases with the increase in temperatures. The obtained values of thermodynamic parameters showed that adsorption of 2,4 DCP is an endothermic process. Synthetic resin was not found efficient to adsorb 2,4 DCP compared to activated carbon. The order of adsorption efficiencies of three resins used in the study found as XAD7HP > XAD4 > XAD1180.

  17. New generation Amberlite XAD resin for the removal of metal ions: A review.

    PubMed

    Ahmad, Akil; Siddique, Jamal Akhter; Laskar, Mohammad Asaduddin; Kumar, Rajeev; Mohd-Setapar, Siti Hamidah; Khatoon, Asma; Shiekh, Rayees Ahmad

    2015-05-01

    The direct determination of toxic metal ions, in environmental samples, is difficult because of the latter's presence in trace concentration in association with complex matrices, thereby leading to insufficient sensitivity and selectivity of the methods used. The simultaneous removal of the matrix and preconcentration of the metal ions, through solid phase extraction, serves as the promising solution. The mechanism involved in solid phase extraction (SPE) depends on the nature of the sorbent and analyte. Thus, SPE is carried out by means of adsorption, ion exchange, chelation, ion pair formation, and so forth. As polymeric supports, the commercially available Amberlite resins have been found very promising for designing chelating matrices due to its good physical and chemical properties such as porosity, high surface area, durability and purity. This review presents an overview of the various works done on the modification of Amberlite XAD resins with the objective of making it an efficient sorbent. The methods of modifications which are generally based on simple impregnation, sorption as chelates and chemical bonding have been discussed. The reported results, including the preconcentration limit, the detection limit, sorption capacity, preconcentration factors etc., have been reproduced.

  18. A model predictive control approach for the Italian LBE XADS

    NASA Astrophysics Data System (ADS)

    Cammi, Antonio; Casella, Francesco; Luzzi, Lelio; Milano, Alessandro; Ricotti, Marco E.

    2008-06-01

    In this paper, model predictive control (MPC) is applied to the Italian 80 MW th experimental accelerator driven system (XADS), referring to a simple, non-linear model for the dynamic simulation of the plant, which has been developed and described in a previous work [A. Cammi, L. Luzzi, A.A. Porta, M.E. Ricotti, Prog. Nucl. Energ. 48 (2006) 578], in order to describe the interactions among the different subsystems: i.e., the accelerator-core coupling, the lead bismuth eutectic (LBE) primary system, the secondary system with diathermic oil and air coolers batteries, which reject the thermal power to the environment. Hereinafter, a model predictive controller is proposed, with the objective to minimize the difference between the average temperature of the diathermic oil and its reference value, while also minimizing the variations of the control input, which is the air coolers mass flow rate. The dynamic response of the LBE-XADS has been evaluated with reference to a reduction of 20% in the reactor power from nominal load conditions: this transient is very demanding for the overall plant, nevertheless the obtained results indicate the effectiveness of the proposed controller.

  19. CTEPP STANDARD OPERATING PROCEDURE FOR PRE-CLEANING FILTERS AND XAD-2 (SOP-5.10)

    EPA Science Inventory

    This SOP summarizes the method for pre-cleaning XAD-2 resin and quartz fiber filters. The procedure provides a cleaning method to help reduce potential background contamination in the resin and filters.

  20. Adsorption of tannic and gallic acids on a new polymeric adsorbent and the effect of Cu(II) on their removal.

    PubMed

    Wang, Jinnan; Li, Aimin; Xu, Li; Zhou, Yang

    2009-09-30

    In this paper, a new polymeric adsorbent WJN-09 for adsorbing and removing tannic and gallic acids from water was prepared, and its adsorption capacities for these two natural organic acids were tested by using the commercial resins XAD-7, XAD-4 and NDA-7 as references. The adsorption capacities of WJN-09 for tannic and gallic acids were higher than those of XAD-4, XAD-7 and NDA-7 at 303 K, which may be attributed to its amino function groups, pore structure and Zeta potential. The adsorption enthalpy changes DeltaH exhibited that the adsorption of tannic acid by WJN-09 was a chemical and endothermic process. Furthermore, batch kinetic studies indicated that the tannic acid adsorbed to WJN-09 could be fitted well by both pseudo-first-order and pseudo-second-order adsorption equations, but the intra-particle diffusion played a dominant role in the adsorption of gallic acid. Changes of resin's Zeta potential and acids' average molecular size were observed when Cu(II) was added in solutions, which could explain the significant increase in WJN-09's adsorption capacity for tannic and gallic acids in the presence of Cu(II).

  1. Liquid chromatographic extraction medium

    DOEpatents

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

    1994-09-13

    A method and apparatus are disclosed for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water. 1 fig.

  2. Liquid chromatographic extraction medium

    DOEpatents

    Horwitz, E. Philip; Dietz, Mark L.

    1994-01-01

    A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

  3. Evaluations of the TiO2/simulated solar UV degradations of XAD fractions of natural organic matter from a bog lake using size-exclusion chromatography.

    PubMed

    Valencia, Sergio; Marín, Juan M; Restrepo, Gloria; Frimmel, Fritz H

    2013-09-15

    This work reports on the changes in compositions of humic acids (HAs) and fulvic acids (FAs) during photocatalytic degradation. The HAs and FAs were obtained from the XAD-resin fractionation of natural-organic matter (NOM) from a bog lake (Lake Hohloh, Black Forest, Germany). Degussa P-25 titanium dioxide (TiO2) in a suspension and a solar UV simulator (batch reactor) were used in the experiments. The photocatalytic degradation of the HAs and FAs were monitored using size-exclusion chromatography (SEC) equipped with dissolved organic carbon (DOC) and ultraviolet (UV254) detection (SEC-DOC and SEC-UV254) and UV-Vis spectrophotometry. The evolutions of the photocatalytic degradations of the HA and FA fractions were selective. The photocatalytic degradation started with the degradations of high molecular weight compounds with relatively high UV254 absorbances in the HA and FA fractions to yield low molecular weight compounds showing less specific UV254 absorbances. Observance of the same tendency for the original NOM from Lake Hohloh indicates that these XAD-fractions still having complex compound mixtures. However, the larger molecular weight fractions of the FAs showed higher preferential adsorptions onto TiO2, which caused their faster degradation rates. Furthermore, FAs showed a greater reduction of the total THM formation potential (TTHMFP) and the organic halogen compounds adsorbable on activated carbon formation potential (AOXFP), in comparison with the HAs.

  4. A comparison of surface water natural organic matter in raw filtered water samples, XAD, and reverse osmosis isolates.

    PubMed

    Maurice, Patricia A; Pullin, Michael J; Cabaniss, Stephen E; Zhou, Qunhui; Namjesnik-Dejanovic, Ksenija; Aiken, George R

    2002-05-01

    This research compared raw filtered waters (RFWs), XAD resin isolates (XAD-8 and XAD-4), and reverse osmosis (RO) isolates of several surface water samples from McDonalds Branch, a small freshwater fen in the New Jersey Pine Barrens (USA). RO and XAD-8 are two of the most common techniques used to isolate natural organic matter (NOM) for studies of composition and reactivity; therefore, it is important to understand how the isolates differ from bulk (unisolated) samples and from one another. Although, any comparison between the isolation methods needs to consider that XAD-8 is specifically designed to isolate the humic fraction, whereas RO concentrates a broad range of organic matter and is not specific to humics. The comparison included for all samples: weight average molecular weight (Mw), number average molecular weight (Mn), polydispersity (rho), absorbance at 280 nm normalized to moles C (epsilon280) (RFW and isolates); and for isolates only: elemental analysis, % carbon distribution by 13C NMR, and aqueous FTIR spectra. As expected, RO isolation gave higher yield of NOM than XAD-8, but also higher ash content, especially Si and S. Mw decreased in the order: RO > XAD-8 > RFW > XAD-4. The Mw differences of isolates compared with RFW may be due to selective isolation (fractionation), or possibly in the case of RO to condensation or coagulation during isolation. 13C NMR results were roughly similar for the two methods, but the XAD-8 isolate was slightly higher in 'aromatic' C and the RO isolate was slightly higher in heteroaliphatic and carbonyl C. Infrared spectra indicated a higher carboxyl content for the XAD-8 isolates and a higher ester:carboxyl ratio for the RO isolates. The spectroscopic data thus are consistent with selective isolation of more hydrophobic compounds by XAD-8, and also with potential ester hydrolysis during that process, although further study is needed to determine whether ester hydrolysis does indeed occur. Researchers choosing between

  5. A comparison of surface water natural organic matter in raw filtered water samples, XAD, and reverse osmosis isolates

    USGS Publications Warehouse

    Maurice, P.A.; Pullin, M.J.; Cabaniss, S.E.; Zhou, Q.; Namjesnik-Dejanovic, K.; Aiken, G.R.

    2002-01-01

    This research compared raw filtered waters (RFWs), XAD resin isolates (XAD-8 and XAD-4), and reverse osmosis (RO) isolates of several surface water samples from McDonalds Branch, a small freshwater fen in the New Jersey Pine Barrens (USA). RO and XAD-8 are two of the most common techniques used to isolate natural organic matter (NOM) for studies of composition and reactivity; therefore, it is important to understand how the isolates differ from bulk (unisolated) samples and from one another. Although, any comparison between the isolation methods needs to consider that XAD-8 is specifically designed to isolate the humic fraction, whereas RO concentrates a broad range of organic matter and is not specific to humics. The comparison included for all samples: weight average molecular weight (Mw), number average molecular weight (Mn), polydispersity (??), absorbance at 280nm normalized to moles C (??280) (RFW and isolates); and for isolates only: elemental analysis, % carbon distribution by 13C NMR, and aqueous FTIR spectra. As expected, RO isolation gave higher yield of NOM than XAD-8, but also higher ash content, especially Si and S. Mw decreased in the order: RO>XAD-8>RFW>XAD-4. The Mw differences of isolates compared with RFW may be due to selective isolation (fractionation), or possibly in the case of RO to condensation or coagulation during isolation. 13C NMR results were roughly similar for the two methods, but the XAD-8 isolate was slightly higher in 'aromatic' C and the RO isolate was slightly higher in heteroaliphatic and carbonyl C. Infrared spectra indicated a higher carboxyl content for the XAD-8 isolates and a higher ester:carboxyl ratio for the RO isolates. The spectroscopic data thus are consistent with selective isolation of more hydrophobic compounds by XAD-8, and also with potential ester hydrolysis during that process, although further study is needed to determine whether ester hydrolysis does indeed occur. Researchers choosing between XAD and RO

  6. The presence of dichloromethane on cleaned XAD-2 resin: A potential problem and solutions

    SciTech Connect

    Chuang, J.C.; Holdren, M.W. ); Wilson, N.K. )

    1990-06-01

    Preparation of XAD-2 resin for indoor air sampling with commonly used cleaning methods, such as Soxhlet extraction with dichloromethane (DCM) followed by vacuum drying and nitrogen purging, can lead to elevated DCM levels (> 100 ppb) in the sampled indoor air, which result from DCM remaining in the resin after cleaning. Since DCM is a suspect human carcinogen, indoor human exposure to DCM should be minimized. Several procedures to remove residual DCM after Soxhlet extraction were evaluated. Removal by fluidizing the XAD-2 resin bed in a drying column with a nitrogen stream at 40{degree}C was best. The effectiveness of this procedure was demonstrated in parallel air sampling with a syringe sampler and with a prototype quiet sampler equipped with a quartz fiber filter and an XAD-2 cartridge in series. Sampling was conducted in an office and in residence. With the modified procedures, indoor DCM levels were at typical indoor values. (< 10 ppb).

  7. Presence of dichloromethane on cleaned XAD-2 resin: A potential problem and solutions

    SciTech Connect

    Chuang, J.C.; Holdren, M.W.; Wilson, N.K.

    1990-01-01

    Preparation of XAD-2 resin for indoor air sampling with commonly used cleaning methods, such as Soxhlet extraction with dichloromethane (DCM) followed by vacuum drying and nitrogen purging, can lead to elevated DCM levels (>100 ppb) in the sampled indoor air, which result from DCM remaining in the resin after cleaning. Since DCM is a suspect human carcinogen, indoor human exposure to DCM should be minimized. Several procedures to remove residual DCM after Soxhlet extraction were evaluated. Removal by fluidizing the XAD-2 resin bed in a drying column with a nitrogen stream at 40C was best. The effectiveness of this procedure was demonstrated in parallel air sampling with a syringe sampler and with a prototype quiet sampler equipped with a quartz fiber filter and an XAD-2 cartridge in series. Sampling was conducted in an office and in residences. With the modified procedures, indoor DCM levels were at typical indoor values (<10 ppb).

  8. 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.

  9. 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.

  10. Effect of the ionic strength of a mobile phase on the chromatographic retention and thermodynamic characteristics of the adsorption of enantiomers of α-phenylcarboxylic acids on a chiral adsorbent with grafted antibiotic eremomycin

    NASA Astrophysics Data System (ADS)

    Reshetova, E. N.

    2017-01-01

    The effect the ionic strength of an aqueous ethanol mobile phase containing buffer salt has the on retention and thermodynamics of adsorption of optical isomers of some α-phenylcarboxylic acids on chiral adsorbent Nautilus-E with grafted antibiotic eremomycin is investigated. It is shown that ion exchange processes participate in the adsorption of enantiomers of α-phenylcarboxylic acids. It is established that electrostatic interactions contribute to the retention of enantiomers of α-phenylcarboxylic acids and affect selectivity only slightly. The dependences of retention characteristics, selectivity, and thermodynamic parameters on the concentration of the buffer salt in the eluent are determined. A statistical analysis of enthalpy-entropy compensation is performed, and the compensation effect is shown to be true. It is found that the points corresponding to the investigated adsorbates are distributed over the compensation dependence according to the spatial structural characteristics of molecules.

  11. Calibration and application of a passive air sampler (XAD-PAS) for volatile methyl siloxanes.

    PubMed

    Krogseth, Ingjerd S; Zhang, Xianming; Lei, Ying D; Wania, Frank; Breivik, Knut

    2013-05-07

    Because the atmosphere is key to understanding the environmental behavior of volatile methyl siloxanes (VMS), a variety of reliable air sampling methods are needed. The purpose of this study was to calibrate and evaluate an existing, polystyrene-divinylbenzene copolymeric resin-based passive air sampler (XAD-PAS) for VMS. Sixteen XAD-PAS were deployed for 7-98 days at a suburban site in Toronto, Canada, while the VMS concentration in air was monitored by an active sampling method. This calibration and a subsequent field test further allowed for investigation of the temporal and spatial variability of VMS in the region. Uptake in the XAD-PAS of octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), and three linear VMS was linear throughout the whole deployment period. Sampling rates were between 0.4 and 0.5 m(3)/day. The XAD-PAS measured ∑VMS concentrations ranged from nondetects in rural areas (n = 3), to 169 ± 49 ng/m(3) in the urban region (n = 21), to levels above 600 ng/m(3) at sewage treatment plants (n = 2). Levels and composition of VMS within the urban area were remarkably uniform in space. Levels, but not composition, were highly variable in time and weakly correlated with temperature, wind speed, and wind direction.

  12. Chromatographic Degradation of Phloridzin

    PubMed Central

    Grochowska, Maria J.

    1966-01-01

    Phloridzin, the main phenolic glucoside in apple leaves, has been found to undergo transformation during chromatography. When chromatographed repeatedly in ammoniacal solvents, at least 2 new derivatives appeared. One of these was identified as phloretic acid. When bioassayed in the presence of indole-3-acetic acid this substance behaved as though it promoted the destruction of the auxin. Comparative bioassay with naphthaleneacetic acid suggested that phloretic acid acts on indoleacetic acid destruction via stimulation of indoleacetic acid oxidase. However, at low concentration and in presence of a small amount of phloridzin it also showed a synergistic effect with indoleacetic acid. A substance with the same characteristics was obtained directly from apple leaves, which are known to contain phloridzin when the extracts were chromatographed only once in the same (alkaline) solvent. While not completely confirmed, this suggests that phloretic acid is normally present in apple leaves, where it may affect growth there by promoting indoleacetic acid oxidation. Images PMID:16656273

  13. Gas chromatograph injection system

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.; Henderson, M. E.; Donaldson, R. W., Jr. (Inventor)

    1975-01-01

    An injection system for a gas chromatograph is described which uses a small injector chamber (available in various configurations). The sample is placed in the chamber while the chamber is not under pressure and is not heated, and there is no chance of leakage caused by either pressure or heat. It is injected into the apparatus by changing the position of a valve and heating the chamber, and is volatilized and swept by a carrier gas into the analysis apparatus.

  14. Application of XAD-4 solid sorbent to the collection of pesticides from water samples: Final report, November 1985-November 1986

    SciTech Connect

    Maskarinec, M.P.; Manning, D.L.

    1987-10-01

    This report summarizes work done to evaluate the efficiency of XAD-4 resin for removing pesticides from water for subsequent analysis. A limited number of pesticides, including lindane, aldrin, and 4,4'-DDT, were added to water, extracted by elution on XAD-4, and analyzed by gas chromatography with electron capture detection. The method was found to be reasonably effective, at least for semiquantitative purposes.

  15. Chromatographic methods of fractionation.

    PubMed

    Friesen, A D

    1987-01-01

    Chromatography's functional versatility, separation efficiency, gentle non-denaturing separating process and ease of automation and scale-up make it attractive for industrial scale protein purification. The Winnipeg Rh Institute's new Plasma Fractionation facility is an example of the use of chromatography for the large scale purification of plasma protein fractions. The fractionation facility has a capacity to process 800 litres of plasma per batch into blood clotting factor VIII and IX, albumin and intravenous immune serum globulin (i.v. ISG). Albumin and i.v. ISG are purified using ion exchange columns of DEAE-Sepharose (230 litre size), DEAE-Biogel (150 litre size) and CM-Sepharose (150 litre size). The chromatographic process is automated using a Modicon 584 Programmable Logic Controller to regulate valves, pumps and sensors which control plasma flow during fractionation. The stainless steel tanks and piping are automatically cleaned-in-place. The high degree of automation and cleaning provides efficient operation and sanitary processing. Chromatographic methods (DEAE-Sepharose and metal chelation) are also being used at the pilot scale to purify the human blood products superoxide dismutase and hemoglobin from outdated red blood cells. Characterization of the protein fractions produced by chromatography has shown them to be of equal or higher quality than fractions produced by other techniques.

  16. AMS radiocarbon age for fossil bone by XAD-2 chromatography method

    NASA Astrophysics Data System (ADS)

    Minami, Masayo; Nakamura, Toshio

    2000-10-01

    The XAD-2 chromatography method was examined for its ability to efficiently eliminate exogenous organic matter from fossil bones and to improve the accuracy of radiocarbon ( 14C) dating and stable isotope determinations on bone proteins. The fossil bones used in the experiment were animal fossil bones collected from the Awazu submarine archaeological site, Shiga, Japan. For comparison, the gelatin-extraction method was also applied to the same samples. It was found that the gelatin-extraction method is sufficient for 14C dating on well-preserved bones, but insufficient on poorly preserved bones, containing less than 1% extractable gelatin. The XAD-2 resin is useful for the clean up of proteins especially from poorly preserved bones. The carbon stable isotope fractionation of around 1‰ by XAD-2 treatment on modern collagen standards was larger than reported previously. The isotopic variation by sequential extraction of bones probably originates from changes in the amino acid composition and seems to be less sensitive to the indication of the removal of organic contamination.

  17. 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.

  18. 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.

  19. Permeabilization and in situ adsorption studies during growth and coumarin production in hairy root cultures of Cichorium intybus L.

    PubMed

    Bais, H P; Sudha, G; Suresh, B; Ravishankar, G A

    2001-06-01

    Effect of addition of a permeabilizing agent dimethyl sulfoxide (DMSO) and a solid adsorbent, XAD -7, on growth and coumarin production in hairy root cultures of C. intybus was studied. Continuous permeabilization of the hairy root cultures of C. intybus with DMSO has been shown to be an effective strategy for enhanced release of coumarins while preserving the root viability. DMSO at 0.2% (v/v) level showed the maximum growth and coumarin production but was less as compared to control on day 28. Treatment of cells with increasing concentrations of DMSO (0.3 - 0.6 % v/v) to hairy root cultures of C. intybus, showed an inverse relationship with growth and coumarin production. Growth and production of coumarins increased with 1% media filtrate (MF) of cultures of Phytopthora parasitica var. nicotiana treatment. It was observed that treatment with DMSO (0.2% v/v) and 1% MF of P. parasitica showed the better growth and coumarin production with an increased release of coumarins as compared to the control and other treatments. It was observed that treatment of hairy root cultures with XAD-7 resulted in lesser growth and coumarin production as compared to control during the culture period. Addition of XAD-7 along with 1% MF of P. parasitica showed enhanced growth, coumarin production and increased adsorption as compared to control and lone XAD-7 treatment. Combined addition of DMSO/XAD-7 with fungal elicitor showed synergistic response in terms of biomass and coumarin production. Excretion of coumarins in both the cases was dependent on the presence of DMSO/XAD-7. These results showed that continuous permeabilization of hairy root cultures of C. intybus by using DMSO at 0.2% (v/v) level coupled with 1% MF of P. parasitica maintained viability of tissues and produced coumarins at higher level.

  20. Multilayer adsorption on fractal surfaces.

    PubMed

    Vajda, Péter; Felinger, Attila

    2014-01-10

    Multilayer adsorption is often observed in liquid chromatography. The most frequently employed model for multilayer adsorption is the BET isotherm equation. In this study we introduce an interpretation of multilayer adsorption measured on liquid chromatographic stationary phases based on the fractal theory. The fractal BET isotherm model was successfully used to determine the apparent fractal dimension of the adsorbent surface. The nonlinear fitting of the fractal BET equation gives us the estimation of the adsorption equilibrium constants and the monolayer saturation capacity of the adsorbent as well. In our experiments, aniline and proline were used as test molecules on reversed phase and normal phase columns, respectively. Our results suggest an apparent fractal dimension 2.88-2.99 in the case of reversed phase adsorbents, in the contrast with a bare silica column with a fractal dimension of 2.54.

  1. Preparation of a novel magnetic microporous adsorbent and its adsorption behavior of p-nitrophenol and chlorotetracycline.

    PubMed

    Ma, Yan; Zhou, Qing; Li, Aimin; Shuang, Chendong; Shi, Qianqian; Zhang, Mancheng

    2014-02-15

    A novel method for fabricating hypercrosslinked magnetic polymer beads with improved acid resistance was developed. Magnetite nanoparticles were covered with tetraethoxysilane and vinyltriethoxysilane, followed by co-polymerization and post-crosslinking. The resulting M150 beads were highly stable at pH ≥ 2 and were superparamagnetic, with a saturation magnetization of 3.1 emu/g. M150 exhibited a specific surface area of 1022.4m(2)/g and an average pore width of 2.6 nm. The adsorption of p-nitrophenol and chlorotetracycline (CTC) onto M150 and the commercial non-magnetic resins NDA 150 and XAD-4 followed both pseudo-first-order and pseudo-second-order equations. M150 displayed much faster kinetics than the other resins because of its small particle size and abundant macropores. The adsorption isotherm of p-nitrophenol onto the three resins fitted the Freundlich equation (R(2)>0.98), whereas CTC adsorption was better described by the Langmuir isotherm. p-Nitrophenol adsorption was optimal at pH ≤ 4, whereas CTC adsorption was optimal at pH 5-6. All three sorbents showed high reusability for p-nitrophenol adsorption. XAD-4 demonstrated the highest reusability for CTC. The CTC adsorption capacities of M150 and NDA150 decreased by 12.42% and 20% after 10 adsorption-desorption cycles, respectively.

  2. Sorption of a diverse set of organic chemical vapors onto XAD-2 resin: Measurement, prediction and implications for air sampling

    NASA Astrophysics Data System (ADS)

    Hayward, Stephen J.; Lei, Ying D.; Wania, Frank

    2011-01-01

    The wide-spread use of styrene-divinylbenzene-copolymeric resin (XAD-2) in air sampling necessitates a quantitative understanding of its sorption characteristics for organic chemicals. Inverse Gas Chromatography (IGC) was used to measure the sorption of a diverse set of 52 organic chemicals to XAD-2 at temperatures between 40 °C and 100 °C and at relative humidities between 0 and 87%. Even though relative humidity has been shown to influence sorption to other sorbents, it did not significantly influence most chemicals' sorption to XAD-2, indicating that water does not form a strong physical barrier to sorption on XAD-2 at high relative humidity. The resin-air partition coefficients ( KXAD) determined by IGC and the enthalpies of sorption derived from them were regressed against solute descriptors to derive poly-parameter Linear Free Energy Relationships (ppLFERs) which allow the estimation of KXAD for chemicals which are not sufficiently volatile to be amenable to IGC and for temperatures outside the experimental range. KXAD values at 20 °C estimated for a set of 296 chemicals for which solute descriptors are available, including polychlorinated biphenyls, polycyclic aromatic hydrocarbons, and pesticides, indicate that for many of the substances commonly found in the atmosphere sorption is higher to XAD-2 than to poly-urethane foam, another popular air sampling sorbent.

  3. Model-based design of peptide chromatographic purification processes.

    PubMed

    Gétaz, David; Stroehlein, Guido; Butté, Alessandro; Morbidelli, Massimo

    2013-04-05

    In this work we present a general procedure for the model-based optimization of a polypeptide crude mixture purification process through its application to a case of industrial relevance. This is done to show how much modeling can be beneficial to optimize complex chromatographic processes in the industrial environment. The target peptide elution profile was modeled with a two sites adsorption equilibrium isotherm exhibiting two inflection points. The variation of the isotherm parameters with the modifier concentration was accounted for. The adsorption isotherm parameters of the target peptide were obtained by the inverse method. The elution of the impurities was approximated by lumping them into pseudo-impurities and by regressing their adsorption isotherm parameters directly as a function of the corresponding parameters of the target peptide. After model calibration and validation by comparison with suitable experimental data, Pareto optimizations of the process were carried out so as to select the optimal batch process.

  4. Quinalizarin anchored on Amberlite XAD-2. A new matrix for solid-phase extraction of metal ions for flame atomic absorption spectrometric determination.

    PubMed

    Kumar, M; Rathore, D P; Singh, A K

    2001-06-01

    Amberlite XAD-2 has been functionalized by coupling it to quinalizarin [1,2,5,8-tetrahydroxyanthraquinone] by means of an -N = N- spacer. Elemental analysis, thermogravimetric analysis, and infrared spectra were used to characterize the resulting new polymer matrix. The matrix has been used to preconcentrate Cu(II), Cd(II), Co(II), Pb(II), Zn(II), and Mn(II) before their determination by flame atomic absorption spectrometry (FAAS). UO2(II) has been preconcentrated for fluorimetric determination. The optimum pH values for maximum adsorption of the metals are between 5.0 and 7.0. All these metal ions are desorbed (recovery 91-99%) with 4 mol L(-1) HNO3. The adsorptive capacity of the resin was found to be in the range 0.94-5.28 mg metal g(-1) resin and loading half-life (t1/2) between 5.3 and 15.0 min. The effects of NaF, NaCl, NaNO3, Na2SO4, Na3PO4, Ca(II), and Mg(II) on the adsorption of these metal ions (0.2 microg mL(-1)) are reported. The lower limits of detection for these metal ions are between 1 and 15.0 microg L(-1). After enrichment on this matrix flame AAS has been used to determine these metal ions (except the uranyl ion) in river water samples (RSD < or = 6.5%); fluorimetry was used to determine uranyl ion in well water samples (RSD < or = 6.3%). Cobalt from pharmaceutical vitamin tablets was preconcentrated by use of this chelating resin and estimated by FAAS (RSD approximately 4%).

  5. XadM, a novel adhesin of Xanthomonas oryzae pv. oryzae, exhibits similarity to Rhs family proteins and is required for optimum attachment, biofilm formation, and virulence.

    PubMed

    Pradhan, Binod B; Ranjan, Manish; Chatterjee, Subhadeep

    2012-09-01

    By screening a transposon-induced mutant library of Xanthomonas oryzae pv. oryzae, the bacterial blight pathogen of rice, we have identified a novel 5.241-kb open reading frame (ORF) named xadM that is required for optimum virulence and colonization. This ORF encodes a protein, XadM, of 1,746 amino acids that exhibits significant similarity to Rhs family proteins. The XadM protein contains several repeat domains similar to a wall-associated surface protein of Bacillus subtilis, which has been proposed to be involved in carbohydrate binding. The role of XadM in X. oryzae pv. oryzae adhesion was demonstrated by the impaired ability of an xadM mutant strain to attach and form biofilms. Furthermore, we show that XadM is exposed on the cell surface and its expression is regulated by growth conditions and plays an important role in the early attachment and entry inside rice leaves. Interestingly, XadM homologs are present in several diverse bacteria, including many Xanthomonas spp. and animal-pathogenic bacteria belonging to Burkholderia spp. This is the first report of a role for XadM, an Rhs family protein, in adhesion and virulence of any pathogenic bacteria.

  6. A mass transfer model for the fixed-bed adsorption of ferulic acid onto a polymeric resin: axial dispersion and intraparticle diffusion.

    PubMed

    Davila-Guzman, Nancy E; Cerino-Córdova, Felipe J; Soto-Regalado, Eduardo; Loredo-Cancino, Margarita; Loredo-Medrano, José A; García-Reyes, Refugio B

    2016-08-01

    In this study, amberlite XAD-16 (XAD-16) bed column system was used to remove ferulic acid (FA) from aqueous solutions. Laboratory-scale column experiments were conducted in downflow fixed bed at initial FA concentration of 1 g/L, initial pH 3, and 25°C. The performance of the adsorbent bed under different flow rates (1.3-7.7 mL/min) was studied. The bed utilization efficiency was in the range of 64.64-72.21% at the studied flow rates. A mass transfer model considering both axial dispersion and intraparticle diffusion was developed to predict the breakthrough curves of FA adsorption on XAD-16. This model predicted the experimental data better than Bohart-Adams model and Thomas model, based on the low deviation between predicted and experimental data. The axial dispersion coefficient value varied from 6.45 × 10(-6) to 1.10 × 10(-6) m(2)/s at flow rate from 1.3 to 7.7 mL/min, whereas the intraparticle diffusion coefficient was 1.04 × 10(-10) m(2)/s, being this last resistance the rate-limiting step. In conclusion, axial dispersion and intraparticle diffusion phenomena play the major role in predicting the adsorption of FA onto XAD-16 in fixed-bed columns.

  7. Simultaneous spectrophotometric determination of trace amounts of uranium, thorium, and zirconium using the partial least squares method after their preconcentration by alpha-benzoin oxime modified Amberlite XAD-2000 resin.

    PubMed

    Ghasemi, Jahan B; Zolfonoun, E

    2010-01-15

    A new solid phase extraction method for separation and preconcentration of trace amounts of uranium, thorium, and zirconium in water samples is proposed. The procedure is based on the adsorption of U(VI), Th(IV) and Zr(IV) ions on a column of Amberlite XAD-2000 resin loaded with alpha-benzoin oxime prior to their simultaneous spectrophotometric determination with Arsenazo III using orthogonal signal correction partial least squares method. The enrichment factor for preconcentration of uranium, thorium, and zirconium was found to be 100. The detection limits for U(VI), Th(IV) and Zr(IV) were 0.50, 0.54, and 0.48microgL(-1), respectively. The precision of the method, evaluated as the relative standard deviation obtained by analyzing a series of 10 replicates, was below 4% for all elements. The practical applicability of the developed sorbent was examined using synthetic seawater, natural waters and ceramic samples.

  8. Synthesis, characterization and adsorption performance of a novel post-crosslinked adsorbent.

    PubMed

    Zeng, Xiaowei; Yao, Hongjie; Ma, Ning; Fan, Yunge; Wang, Chunhong; Shi, Rongfu

    2011-02-01

    In this paper a post-crosslinked polymeric adsorbent PDHT-2 with high specific surface area was prepared by Friedel-Crafts reaction of the pendant vinyl groups without an externally added crosslinking agent. It was obvious that both the specific surface area and the pore volume of starting copolymer PDHT-1 increased significantly after post-crosslinking. Batch adsorption runs of phenol from aqueous solution onto adsorbent PDHT-1 and PDHT-2 were researched, and commercial macroporous resin XAD-4 was chosen for comparison purpose. Experimental results showed that the adsorption isotherms could be fitted by Langmuir model and Freundlich model and the adsorption capacity onto PDHT-2 was much larger than that onto PDHT-1 and XAD-4 with respect to phenol and phenolic compound, which possibly resulted from its larger specific surface area. The adsorption process for phenol onto the three adsorbents was proved to be exothermic and spontaneous in nature. The thermodynamic parameters such as Gibb's free energy (ΔG), change in enthalpy (ΔH) and change in entropy (ΔS) had been calculated. The adsorption kinetic curves obeyed the pseudo-second order model and the intraparticle diffusion process was the rate-controlling step.

  9. Isolation of organic acids from large volumes of water by adsorption on macroporous resins

    USGS Publications Warehouse

    Aiken, George R.; Suffet, I.H.; Malaiyandi, Murugan

    1987-01-01

    Adsorption on synthetic macroporous resins, such as the Amberlite XAD series and Duolite A-7, is routinely used to isolate and concentrate organic acids from forge volumes of water. Samples as large as 24,500 L have been processed on site by using these resins. Two established extraction schemes using XAD-8 and Duolite A-7 resins are described. The choice of the appropriate resin and extraction scheme is dependent on the organic solutes of interest. The factors that affect resin performance, selectivity, and capacity for a particular solute are solution pH, resin surface area and pore size, and resin composition. The logistical problems of sample handling, filtration, and preservation are also discussed.

  10. N-benzoyl-n-phenylhydroxylamine impregnated Amberlite XAD-4 beads for selective removal of thorium.

    PubMed

    Chandramouleeswaran, S; Ramkumar, Jayshree

    2014-09-15

    n-Benzoyl-n-phenylhydroxylamine impregnated Amberlite XAD-4 beads were used for the removal of Th(IV) from a mixture of ions. The impregnated XAD was characterized using different techniques like weight and colour change, IR spectra, surface area and pore size measurements to confirm the presence of n-BPHA within the macroreticular resin structure. The experimental conditions were optimized to make the separation fast and selective. It was seen that the maximum sorption was achieved in the pH range of 3-7.5 and uptake was nearly complete within half an hour. The results obtained in the present study were subjected to extensive modelling in order to get a complete understanding of the sorption process. It is seen that the maximum uptake was calculated to be 500 mg/g and has very fast kinetics it was seen that the process is chemisorption. It was further deduced from the modelling that the overall sorption process was controlled dominantly by external mass transfer. Considering the simplicity this procedure, the present study has a possible application for the removal of thorium from different mixtures.

  11. Radioimmunological screening and gas chromatographic determination of morphine and related narcotic analgesics in post mortem blood.

    PubMed

    Cimbura, G; Koves, E

    1981-01-01

    A sensitive, reproducible, and relatively specific procedure is presented for the screening, identification, and quantitation of morphine, hydromorphone, codeine, oxycodone, and hydrocodone in autopsy blood. The drugs are isolated from whole blood by adsorption on an XAD-2 resin slurry and subsequent elution with an organic solvent mixture. Part of the resin extract is screened for morphine and related cross-reacting compounds by a commercially available radioimmunoassay (RIA) and the remainder of the same extract is analyzed by gas chromatography using a nitrogen/phosphorus detector (GC/NP). The procedure has been used frequently in forensic toxicological casework. Since toxic blood concentrations of hydrocodone have not been well documented, the results of toxicological examination of two fatalities involving this drug are presented.

  12. Dual liquid and gas chromatograph system

    DOEpatents

    Gay, D.D.

    A chromatographic system is described that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a nontransparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extreme low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

  13. Dual liquid and gas chromatograph system

    DOEpatents

    Gay, Don D.

    1985-01-01

    A chromatographic system that utilizes one detection system for gas chromatographic and micro-liquid chromatographic determinations. The detection system is a direct-current, atmospheric-pressure, helium plasma emission spectrometer. The detector utilizes a non-transparent plasma source unit which contains the plasma region and two side-arms which receive effluents from the micro-liquid chromatograph and the gas chromatograph. The dual nature of this chromatographic system offers: (1) extreme flexibility in the samples to be examined; (2) extremely low sensitivity; (3) element selectivity; (4) long-term stability; (5) direct correlation of data from the liquid and gas samples; (6) simpler operation than with individual liquid and gas chromatographs, each with different detection systems; and (7) cheaper than a commercial liquid chromatograph and a gas chromatograph.

  14. Deconvolution of gas chromatographic data

    NASA Technical Reports Server (NTRS)

    Howard, S.; Rayborn, G. H.

    1980-01-01

    The use of deconvolution methods on gas chromatographic data to obtain an accurate determination of the relative amounts of each material present by mathematically separating the merged peaks is discussed. Data were obtained on a gas chromatograph with a flame ionization detector. Chromatograms of five xylenes with differing degrees of separation were generated by varying the column temperature at selected rates. The merged peaks were then successfully separated by deconvolution. The concept of function continuation in the frequency domain was introduced in striving to reach the theoretical limit of accuracy, but proved to be only partially successful.

  15. Preliminary numerical analysis of improved gas chromatograph model

    NASA Technical Reports Server (NTRS)

    Woodrow, P. T.

    1973-01-01

    A mathematical model for the gas chromatograph was developed which incorporates the heretofore neglected transport mechanisms of intraparticle diffusion and rates of adsorption. Because a closed-form analytical solution to the model does not appear realizable, techniques for the numerical solution of the model equations are being investigated. Criteria were developed for using a finite terminal boundary condition in place of an infinite boundary condition used in analytical solution techniques. The class of weighted residual methods known as orthogonal collocation is presently being investigated and appears promising.

  16. Purification of olive mill wastewater phenols through membrane filtration and resin adsorption/desorption.

    PubMed

    Zagklis, Dimitris P; Vavouraki, Aikaterini I; Kornaros, Michael E; Paraskeva, Christakis A

    2015-03-21

    Olive tree cultivation has a long history in the Mediterranean countries, and even today consists an important cultural, economic, and environmental aspect of the area. The production of olive oil through 3-phase extraction systems, leads to the co-production of large quantities of olive mill wastewater (OMW), with toxic compounds that inhibit its biodegradation. Membrane filtration has been used for the exploitation of this byproduct, through the isolation of valuable phenolic compounds. In the current work, a fraction of the waste occurring from a membrane process was used. More specifically the reverse osmosis concentrate, after a nanofiltration, containing the low-molecular-weight compounds, was further treated with resin adsorption/desorption. The non ionic XAD4, XAD16, and XAD7HP resins were implemented, for the recovery of phenols and their separation from carbohydrates. The recovered phenolic compounds were concentrated through vacuum evaporation reaching a final concentration of 378 g/L in gallic acid equivalents containing 84.8 g/L hydroxytyrosol.

  17. Synthesis, characterization and adsorption properties of diethylenetriamine-modified hypercrosslinked resins for efficient removal of salicylic acid from aqueous solution.

    PubMed

    Huang, Jianhan; Jin, Xiaoying; Mao, Jinglin; Yuan, Bin; Deng, Rujie; Deng, Shuguang

    2012-05-30

    We report an effective approach for tailoring the pore textural properties and surface polarity of a hypercrosslinked resin to enhance its adsorption capacity and selectivity for removing salicylic acid from aqueous solution. Four hypercrosslinked resins were synthesized by controlling the reaction time of the self Friedel-Crafts reaction of chloromethylated polystyrene-co-divinylbenzene, and then modified with diethylenetriamine to adjust their surface polarity. The resins were characterized with N(2) adsorption for pore textural properties, Fourier transform infrared spectroscopy (FT-IR) for surface functional groups, chemical analysis for residual chlorine content and weak basic exchange capacity. Adsorption equilibrium, kinetics and breakthrough performance were determined for the removal of salicylic acid from aqueous solution on a selected resin HJ-M01. The equilibrium adsorption capacity of salicylic acid on HJ-M01 is significantly higher than that on its precursor HJ-11 and a few commercial adsorbents including AB-8, XAD-4 and XAD-7. The dynamic adsorption capacity of salicylic acid on HJ-M01 was found to be 456.4 mg/L at a feed concentration of 1000 mg/L and 294 K. The used resin could be fully regenerated with 1% sodium hydroxide solution. The hypercrosslinked resins being developed were promising alternatives to commercial adsorbents for removing salicylic acid and other volatile organic compounds (VOCs) from aqueous solution.

  18. Ask the experts: chromatographic baselines.

    PubMed

    Smith, Graeme; James, Christopher A; Scott, Rebecca; Woolf, Eric

    2014-05-01

    Bioanalysis invited a selection of leading researchers to express their views on chromatographic baseline assignment in the bioanalytical laboratory. The topics discussed include the challenges presented with ensuring automated baseline assignment is correct, when reintegration is necessary, regulation and consistency in terminology. Their enlightening responses provide a valuable insight into developing an industry consensus towards reintegration. An accompanying commentary article in this issue, authored by Howard Hill and colleagues (Huntingdon Life Sciences), provides background to this much debated topic.

  19. Application of XAD-resin based passive air samplers to assess local (roadside) and regional patterns of persistent organic pollutants.

    PubMed

    Barthel, Paul; Thuens, Sabine; Shunthirasingham, Chubashini; Westgate, John N; Wania, Frank; Radke, Michael

    2012-07-01

    We used XAD-resin based passive air samplers (PAS) to measure atmospheric levels of polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) at five ombrotrophic bogs in Eastern Canada. The aims of our study were to investigate the influence of local roads on contaminant levels in the bogs, to derive the regional pattern of atmospheric concentrations, and to assess the uncertainties of the method. Expanded uncertainties based on the duplicate PAS deployed at 24 sites were good for the PAHs, while the deployment period of approx. 100 days was too short to yield acceptable uncertainties for PCBs. The regional PAH distribution was in good agreement with the calculated source proximity of the sampled bogs. We conclude that XAD-resin based PAS deployed for comparatively short periods are well suited for measuring atmospheric concentrations of volatile PAHs, while in remote regions longer deployment is necessary for less volatile PAHs and for PCBs.

  20. A Simplified Method for Sampling and Analysis of High Volume Surface Water for Organic Contaminants Using XAD-2

    USGS Publications Warehouse

    Datta, S.; Do, L.V.; Young, T.M.

    2004-01-01

    A simple compressed-gas driven system for field processing and extracting water for subsequent analyses of hydrophobic organic compounds is presented. The pumping device is a pneumatically driven pump and filtration system that can easily clarify at 4L/min. The extraction device uses compressed gas to drive filtered water through two parallel XAD-2 resin columns, at about 200 mL/min. No batteries or inverters are required for water collection or processing. Solvent extractions were performed directly in the XAD-2 glass columns. Final extracts are cleaned-up on Florisil cartridges without fractionation and contaminants analyzed by GC-MS. Method detection limits (MDLs) and recoveries for dissolved organic contaminants, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and pesticides are reported along with results of surface water analysis for the San Francisco Bay, CA.

  1. Comparison of the mutagenic activity of XAD4 and blue rayon extracts of surface water and related drinking water samples.

    PubMed

    Kummrow, Fábio; Rech, Celia M; Coimbrão, Carlos A; Roubicek, Deborah A; Umbuzeiro, Gisela de A

    2003-11-10

    The combination of mutagenicity tests and selective extraction methodologies can be useful to indicate the possible classes of genotoxic organic contaminants in water samples. Treated and source water samples from two sites were analyzed: a river under the influence of an azo dye-processing plant discharge and a reservoir not directly impacted with industrial discharges, but contaminated with untreated domestic sewage. Organic extraction was performed in columns packed with XAD4 resin, that adsorbs a broad class of mutagenic compounds like polycyclic aromatic hydrocarbons (PAHs), arylamines, nitrocompounds, quinolines, antraquinones, etc., including the halogenated disinfection by-products; and with blue rayon that selectively adsorbs polycyclic planar structures. The organic extracts were tested for mutagenicity with the Salmonella assay using TA98 and TA100 strains and the potencies were compared. A protocol for cleaning the blue rayon fibers was developed and the efficiency of the reused fibers was analyzed with spiked samples. For the river water samples under the influence of the azo-type dye-processing plant, the mutagenicity was much higher for both blue rayon and XAD4 extracts when compared to the water from the reservoir not directly impacted with industrial discharges. For the drinking water samples, although both sites showed mutagenic responses with XAD4, only samples from the site under the influence of the industrial discharge showed mutagenic activity with the blue rayon extraction, suggesting the presence of polycyclic compounds in those samples. As expected, negative results were found with the blue rayon extracts of the drinking water collected from the reservoir not contaminated with industrial discharges. In this case, it appears that using the blue rayon to extract drinking water samples and comparing the results with the XAD resin extracts we were able to distinguish the mutagenicity caused by industrial contaminants from the halogenated

  2. Regulation of isoflavone production in hydroponically grown Pueraria montana (kudzu) by cork pieces, XAD-4, and methyl jasmonate.

    PubMed

    Kirakosyan, Ara; Kaufman, Peter B; Chang, Soo Chul; Warber, Sara; Bolling, Steven; Vardapetyan, Hrachik

    2006-12-01

    A mini-hydroponic growing system was employed for seedlings of kudzu vine (Pueraria montana) and contents of isoflavones (daidzein, genistein, daidzin, genistin, and puerarin) from shoot and root parts of seedlings were analyzed quantitatively. In addition, exogenous cork pieces, polymeric adsorbent, XAD-4, and universal elicitor, methyl jasmonate (MeJA), were used to regulate the production of these isoflavones. It was shown that cork pieces up-regulate the production of daidzein and genistein up to seven- and eight-fold greater than the levels obtained for control roots. In contrast, levels of glucosyl conjugates, daidzin and genistin, decrease up to five- and eight-fold, respectively. Cork treatment also induces the excretion of the root isoflavone constituents into the growth medium. Minimal levels of isoflavones are absorbed by the cork pieces. XAD-4 stimulates the production of glucosyl conjugates, daidzin and genistin, in root parts about 1.5-fold greater than that obtained in control roots. These are the highest amounts of daidzin and genistin that are observed (5.101 and 6.759 mg g(-1) dry weight, respectively). In contrast to these two adsorbents, MeJA increases the accumulation of isoflavones in shoot rather than in root parts of seedlings, about three- to four-fold over control levels, with the exception of genistein. These studies reveal new observations on the regulation of isoflavone production in hydroponically grown Pueraria montana plants by two adsorbents (cork pieces and XAD-4) and MeJA elicitor.

  3. Vibrational Spectroscopy of Chromatographic Interfaces

    SciTech Connect

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  4. Transesterification of propylene glycol methyl ether in chromatographic reactors using anion exchange resin as a catalyst.

    PubMed

    Oh, Jungmin; Sreedhar, Balamurali; Donaldson, Megan E; Frank, Timothy C; Schultz, Alfred K; Bommarius, Andreas S; Kawajiri, Yoshiaki

    2016-09-30

    Reactive chromatography using an anion exchange resin is proposed for a transesterification reaction of propylene glycol methyl ether (DOWANOL™ PM) with ethyl acetate to produce propylene glycol methyl ether acetate (DOWANOL™ PMA). This reaction is studied in batch and chromatographic reactors catalyzed by an anion exchange resin. Several anion exchange resins are tested and compared based on the performance of resin as an adsorbent and a catalyst. A chromatographic column is packed with a selected catalyst, AMBERLITE™ IRA904, and both reaction and chromatographic elution are studied at different temperatures and feed concentrations. The resulting chromatograms are fitted to a mathematical model to obtain adsorption equilibrium and reaction kinetic parameters by the inverse method. Compared to esterification investigated in a previous study, transesterification has advantages such as a higher conversion at lower temperature and easy removal of the byproduct which may lead to higher productivity. Deactivation of anion exchange resins is observed and potential solutions are suggested.

  5. Experimental adsorption isotherms based on inverse gas chromatography.

    PubMed

    Kalogirou, E; Bassiotis, I; Artemiadi, Th; Margariti, S; Siokos, V; Roubani-Kalantzopoulou, F

    2002-09-06

    A new chromatographic perturbation method is used for studying the adsorption-desorption equilibrium in various gas-solid heterogeneous systems. It is the reversed-flow method giving accurate and precise values of many physicochemical constants including the basic and necessary adsorption isotherm values. For four inorganic oxides, namely, Cr2O3, Fe2O3, TiO2 and PbO, and two aromatic hydrocarbons (benzene, toluene) these adsorption isotherms have been determined through a non-linear model.

  6. Enhanced adsorption of phenol from water by a novel polar post-crosslinked polymeric adsorbent.

    PubMed

    Zeng, Xiaowei; Fan, Yunge; Wu, Guolin; Wang, Chunhong; Shi, Rongfu

    2009-09-30

    A novel post-crosslinked polymeric adsorbent PDM-2 was prepared by Friedel-Crafts reaction of pendant vinyl groups without external crosslinking agent. Both the specific surface area and the pore volume of starting copolymer PDM-1 increased significantly after post-crosslinking. Batch adsorption runs of phenol from aqueous solution onto PDM-1 and PDM-2 were investigated. Commercial macroporous resins XAD-4 and AB-8 were chosen as the comparison. Experimental results showed that isotherms of phenol adsorption onto these four polymeric adsorbents could be represented by Freundlich model reasonably. PDM-2 exhibited higher adsorption capacity of phenol than other three adsorbents, which resulted from synergistic effect of larger specific surface area and polar groups on the network. The adsorption process for phenol was proved to be exothermic and spontaneous in nature. Thermodynamic parameters such as Gibb's free energy (DeltaG), change in enthalpy (DeltaH) and change in entropy (DeltaS) were calculated. Kinetics studies indicated that phenol uptake onto PDM-1 and PDM-2 followed the pseudo-second order model and the intraparticle diffusion process was a rate-controlling step. Column adsorption runs demonstrated that nearly 100% regeneration efficiency for PDM-2 by 3BV industrial alcohol and the adsorbate phenol can be easily recovered by further distilling. Continuous column adsorption-regeneration cycles indicated negligible capacity loss of PDM-2 during operation.

  7. Gas Chromatographic Determination of Enrivonmentally Significant Pesticides.

    ERIC Educational Resources Information Center

    Rudzinski, Walter E.; Beu, Steve

    1982-01-01

    A chromatographic procedure for analyzing organophosphorus pesticides (such as PCB's, nitrosamines, and phthalate esters) in orange juice is described, including a summary of the method, instrumentation, methodology, results/discussion, and calculations. (JN)

  8. A Versatile, Automatic Chromatographic Column Packing Device

    ERIC Educational Resources Information Center

    Barry, Eugene F.; And Others

    1977-01-01

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

  9. A Quantitative Gas Chromatographic Ethanol Determination.

    ERIC Educational Resources Information Center

    Leary, James J.

    1983-01-01

    Describes a gas chromatographic experiment for the quantitative determination of volume percent ethanol in water ethanol solutions. Background information, procedures, and typical results are included. Accuracy and precision of results are both on the order of two percent. (JN)

  10. Radiocarbon, 13C and 15N analysis of fossil bone: Removal of humates with XAD-2 resin

    NASA Astrophysics Data System (ADS)

    Stafford, Thomas W., Jr.; Brendel, Klaus; Duhamel, Raymond C.

    1988-09-01

    Humic acids are the predominant source of error in the 14C and stable isotope analysis of fossil bone organic matter. XAD-2 resin will quantitatively remove humates and give the highest yields of protein from bones with variable types of preservation. Decalcified bone, gelatin and base-leached residues can vary up to 5%. for δ 13C and by 1%. on δ 15N relative to XAD-treated fractions. Simultaneous analysis of 14C age, δ 13C and δ 15N is recommended because each isotope value can be independently affected by the bone's diagenetic history. Radiocarbon analysis is the most sensitive and δ 15N is least sensitive for detecting exogenous organic matter. The uncertainty of analyses on the best pretreated protein is ±0.5%. for both δ 13C and δ 15N and is larger than previous estimates. The accuracy for all isotope analyses will be better assessed by using individual amino acids instead of total collagenous residues. Inaccurate 14C dates on severely degraded bone are an indication that this class of fossils may be unsuitable for any isotopic analysis.

  11. Nanofluidic Size-Exclusion Chromatograph

    NASA Technical Reports Server (NTRS)

    Feldman, Sabrina; Svehla, Danielle; Grunthaner, Frank; Feldman, Jason; Shakkottai, P.

    2004-01-01

    Efforts are under way to develop a nanofluidic size-exclusion chromatograph (SEC), which would be a compact, robust, lightweight instrument for separating molecules of interest according to their sizes and measuring their relative abundances in small samples. About as large as a deck of playing cards, the nanofluidic SEC would serve, in effect, as a laboratory on a chip that would perform the functions of a much larger, conventional, bench-top SEC and ancillary equipment, while consuming much less power and much smaller quantities of reagent and sample materials. Its compactness and low power demand would render it attractive for field applications in which, typically, it would be used to identify and quantitate a broad range of polar and nonpolar organic compounds in soil, ice, and water samples. Size-exclusion chromatography is a special case of high-performance liquid chromatography. In a conventional SEC, a sample plug is driven by pressure along a column packed with silica or polymer beads that contain uniform nanopores. The interstices between, and the pores in, the beads collectively constitute a size-exclusion network. Molecules follow different paths through the size-exclusion network, such that characteristic elution times can be related to sizes of molecules: basically, smaller molecules reach the downstream end of the column after the larger ones do because the smaller ones enter minor pores and stay there for a while, whereas the larger ones do not enter the pores. The volume accessible to molecules gradually diminishes as their size increases. All molecules bigger than a pore size elute together. For most substances, the elution times and sizes of molecules can be correlated directly with molecular weights. Hence, by measuring the flux of molecules arriving at the downstream end as a function of time, one can obtain a liquid mass spectrum for the molecules present in a sample over a broad range of molecular weights.

  12. Characterization and evaluation of a macroporous adsorbent for possible use in the expanded bed adsorption of flavonoids from Ginkgo biloba L.

    PubMed

    Li, Jing; Chase, Howard A

    2009-12-11

    The suitability of the use of macroporous adsorbent Amberlite XAD7HP in expanded bed adsorption processes for the isolation of flavonoids from crude extracts of Ginkgo biloba L. has been assessed. The expansion and hydrodynamic properties of expanded beds were investigated and analyzed. The bed expansion as a function of operational fluid velocity was measured and correlated with the Richardson-Zaki equation. Theoretical predictions of the correlation parameters (the terminal settling velocity u(t) and exponent n) were improved by modifying equations in the literature. Residence time distributions (RTDs) were studied using acetone as a tracer. Three measures of liquid phase dispersion (the height equivalent of theoretical plate, Bodenstein number and axial distribution coefficient) were investigated and compared to values previously obtained with commercial EBA adsorbents developed for protein purification. A suitable bed expansion ratio was found to be 1.25 times the settled bed height, which occurred at a corresponding flow velocity of 183 cm/h. For an initial settled bed height of 42 cm, the mean residence time of liquid in the expanded bed was around 28 min. Under these flow conditions, the axial mixing coefficient D(ax) was 7.54 x 10(-6) m(2)/s and the Bodenstein number was 28; the number of theoretical plates (N) was 19 and the height equivalent of a theoretical plate (HETP) was 2.77 cm. Rutin trihydrate was used as a model flavonoid for the characterization of the adsorption properties of Amberlite XAD7HP. Adsorption was observed to reach equilibrium within 3 h with 70% of the adsorption capacity being achieved within 30 min. The estimated maximum equilibrium adsorption capacity for rutin was estimated to be 43.0 mg/(gresin) when the results were fitted to Langmuir isotherms. The adsorption performance was not seriously impaired by the physical presence of G. biloba leaf powders. Assessment of the kinetics of the adsorption of rutin revealed that the rate

  13. Comparison of XAD with other dissolved lignin isolation techniques and a compilation of analytical improvements for the analysis of lignin in aquatic settings

    USGS Publications Warehouse

    Spencer, Robert G. M.; Aiken, George R.; Dyda, Rachael Y.; Butler, Kenna; Bergamaschi, Brian; Hernes, Peter J.

    2010-01-01

    This manuscript highlights numerous incremental improvements in dissolved lignin measurements over the nearly three decades since CuO oxidation of lignin phenols was first adapted for environmental samples. Intercomparison of the recovery efficiency of three common lignin phenol concentration and isolation techniques, namely XAD, C18with both CH3OH (C18M) and CH3CN (C18A) used independently for priming and elution steps, and tangential flow filtration (TFF) for a range of aquatic samples including fresh, estuarine and marine waters, was undertaken. With freshwater samples XAD8-1, C18M and TFF were all observed to recover ca. 80–90% of the lignin phenols and showed no fractionation effects with respect to diagnostic lignin parameters. With estuarine and marine samples more lignin phenols were recovered with C18M and XAD8-1 than TFF because of the increased prevalence of low molecular weight lignin phenols in marine influenced samples. For marine systems, differences were also observed between diagnostic lignin parameters isolated via TFF vs. C18M and XAD8-1 as a result of the high molecular weight lignin phenols being less degraded than the bulk. Therefore, it is recommended for future studies of marine systems that only one technique is utilized for ease of intercomparison within studies. It is suggested that for studies solely aimed at recovering bulk dissolved lignin in marine environments that C18M and XAD8-1 appear to be more suitable than TFF as they recover more lignin. Our results highlight that, for freshwater samples, all three common lignin phenol concentration and isolation techniques are comparable to whole water concentrated by rotary evaporation (i.e. not isolated) but, that for marine systems, the choice of concentration and isolation techniques needs to be taken into consideration with respect to both lignin concentration and diagnostic parameters. Finally, as the study highlights XAD8-1 to be a suitable method for the isolation of dissolved

  14. Comparison of XAD with other dissolved lignin isolation techniques and a compilation of analytical improvements for the analysis of lignin in aquatic settings

    USGS Publications Warehouse

    Spencer, R.G.M.; Aiken, G.R.; Dyda, R.Y.; Butler, K.D.; Bergamaschi, B.A.; Hernes, P.J.

    2010-01-01

    This manuscript highlights numerous incremental improvements in dissolved lignin measurements over the nearly three decades since CuO oxidation of lignin phenols was first adapted for environmental samples. Intercomparison of the recovery efficiency of three common lignin phenol concentration and isolation techniques, namely XAD, C18 with both CH3OH (C18M) and CH3CN (C18A) used independently for priming and elution steps, and tangential flow filtration (TFF) for a range of aquatic samples including fresh, estuarine and marine waters, was undertaken. With freshwater samples XAD8-1, C18M and TFF were all observed to recover ca. 80-90% of the lignin phenols and showed no fractionation effects with respect to diagnostic lignin parameters. With estuarine and marine samples more lignin phenols were recovered with C18M and XAD8-1 than TFF because of the increased prevalence of low molecular weight lignin phenols in marine influenced samples. For marine systems, differences were also observed between diagnostic lignin parameters isolated via TFF vs. C18M and XAD8-1 as a result of the high molecular weight lignin phenols being less degraded than the bulk. Therefore, it is recommended for future studies of marine systems that only one technique is utilized for ease of intercomparison within studies. It is suggested that for studies solely aimed at recovering bulk dissolved lignin in marine environments that C18M and XAD8-1 appear to be more suitable than TFF as they recover more lignin. Our results highlight that, for freshwater samples, all three common lignin phenol concentration and isolation techniques are comparable to whole water concentrated by rotary evaporation (i.e. not isolated) but, that for marine systems, the choice of concentration and isolation techniques needs to be taken into consideration with respect to both lignin concentration and diagnostic parameters. Finally, as the study highlights XAD8-1 to be a suitable method for the isolation of dissolved lignin

  15. Reproductive responses of male fathead minnows exposed to wastewater treatment plant effluent, effluent treated with XAD8 resin, and an environmentally relevant mixture of alkylphenol compounds

    USGS Publications Warehouse

    Barber, L.B.; Lee, K.E.; Swackhamer, D.L.; Schoenfuss, H.L.

    2007-01-01

    On-site, continuous-flow experiments were conducted during August and October 2002 at a major metropolitan wastewater treatment plant (WWTP) to determine if effluent exposure induced endocrine disruption as manifested in the reproductive competence of sexually mature male fathead minnows (Pimephales promelas). The fathead minnows were exposed in parallel experiments to WWTP effluent and WWTP effluent treated with XAD8 macroreticular resin to remove the hydrophobic-neutral fraction which contained steroidal hormones, alkylphenolethoxylates (APEs), and other potential endocrine disrupting compounds (EDCs). The effluent composition varied on a temporal scale and the continuous-flow experiments captured the range of chemical variability that occurred during normal WWTP operations. Exposure to WWTP effluent resulted in vitellogenin induction in male fathead minnows, with greater response in October than in August. Concentrations of ammonia, APEs, 17??-estradiol, and other EDCs also were greater in October than in August, reflecting a change in effluent composition. In the October experiment, XAD8 treatment significantly reduced vitellogenin induction in the male fathead minnows relative to the untreated effluent, whereas in August, XAD8 treatment had little effect. During both experiments, XAD8 treatment removed greater than 90% of the APEs. Exposure of fish to a mixture of APEs similar in composition and concentration to the WWTP effluent, but prepared in groundwater and conducted at a separate facility, elicited vitellogenin induction during both experiments. There was a positive relation between vitellogenin induction and hepatosomatic index (HSI), but not gonadosomatic index (GSI), secondary sexual characteristics index (SSCI), or reproductive competency. In contrast to expectations, the GSI and SSCI increased in males exposed to WWTP effluent compared to groundwater controls. The GSI, SSCI, and reproductive competency were positively affected by XAD8 treatment of

  16. Comparison among three anion exchange chromatographic supports to capture erythropoietin from cell culture supernatant.

    PubMed

    Hernández, Lourdes; Stewart, Diobel; Zumalacárregui, Lourdes; Amaro, Daniel

    2015-06-01

    Affinity and ion exchange conventional chromatography have been used to capture erythropoietin (EPO) from mammalian cell culture supernatant. Currently, chromatographic adsorbent perfusion is available, however a limited number of applications have been found in the literature. In this work, three anion exchange chromatographic supports (gel, membrane and monolithic) were evaluated in the capture step of the recombinant erythropoietin purification process. The influences of load and flow rate on each support performance were analyzed. Also the purity of the EPO molecules was determined. A productivity analysis, as a decision tool for larger scale implementation, was done. As a conclusion, the evaluated supports are technically suitable to capture EPO with adequate recovery and good purity. However, the monolithic column admits high operating velocity, showing the highest adsorption capacity and productivity.

  17. Lumped parameter model for prediction of initial breakthrough profiles for the chromatographic capture of antibodies from a complex feedstock.

    PubMed

    Bak, Hanne; Thomas, Owen R T; Abildskov, Jens

    2007-03-15

    A simple mathematical model to predict initial breakthrough profiles from preparative chromatographic separations of biological macromolecules has been developed. A lumped parameter approach was applied, employing Langmuirian adsorption kinetics to describe the rate of mass transfer (MT) from the bulk liquid in the column to the bound state. Equilibrium and kinetic adsorption data were determined for six different packed bed chromatographic adsorbents: two derivatised with rProtein A; and four functionalised with synthetic low molecular weight ligands. All adsorption isotherms were well described by the Langmuir model, whereas the data fitting to kinetic batch experiments showed that the model was inadequate after the first approximately 25 min of adsorption for four of the six adsorbents. The model underestimated the dynamic Ig breakthough on packed beds of rProtein A Sepharose FF, MabSelect, MBI HyperCel, and MabSorbent A1P, applying a feedstock of 20-100% (v/v) clarified rabbit antiserum. However, when employing a maximum adsorption capacity 25% greater than that determined in batch binding studies, excellent agreement was obtained at all antiserum strengths for most adsorbents. Useful insights into scale-up and process design can be obtained by applying the model, without determining tentative parameters specific for each adsorbent and target protein concentration. However, the model parameters are solvent dependent so a prerequisite for its true applicability is that binding is both Langmuirian and essentially independent of the ionic strength of the feedstock applied.

  18. Portable gas chromatograph-mass spectrometer

    DOEpatents

    Andresen, Brian D.; Eckels, Joel D.; Kimmons, James F.; Myers, David W.

    1996-01-01

    A gas chromatograph-mass spectrometer (GC-MS) for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units.

  19. Portable gas chromatograph-mass spectrometer

    DOEpatents

    Andresen, B.D.; Eckels, J.D.; Kimmons, J.F.; Myers, D.W.

    1996-06-11

    A gas chromatograph-mass spectrometer (GC-MS) is described for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units. 4 figs.

  20. Portable gas chromatograph-mass spectrometer

    SciTech Connect

    Andresen, B.D.; Eckels, J.D.; Kimmins, J.F.; Myers, D.W.

    1994-12-31

    A gas chromatograph-mass spectrometer (GC-MS) for use as a field portable organic chemical analysis instrument. The GC-MS is designed to be contained in a standard size suitcase, weighs less than 70 pounds, and requires less than 600 watts of electrical power at peak power (all systems on). The GC-MS includes: a conduction heated, forced air cooled small bore capillary gas chromatograph, a small injector assembly, a self-contained ion/sorption pump vacuum system, a hydrogen supply, a dual computer system used to control the hardware and acquire spectrum data, and operational software used to control the pumping system and the gas chromatograph. This instrument incorporates a modified commercial quadrupole mass spectrometer to achieve the instrument sensitivity and mass resolution characteristic of laboratory bench top units.

  1. Monitoring of polycyclic aromatic hydrocarbons (PAHs) in the atmosphere of southern Luxembourg using XAD-2 resin-based passive samplers.

    PubMed

    Schummer, Claude; Appenzeller, Brice M; Millet, Maurice

    2014-02-01

    XAD-2 resin-based passive samplers (PAS) with dimensions adapted to 100 mL accelerated solvent extraction cells were used to study the temporal and spatial variations of 17 PAHs on five sites in the atmosphere of southern Luxembourg. This new design allowed extracting the PAS without emptying the resin from the shelter. PAH analyses were done with gas chromatography-tandem mass spectrometry. PAS were deployed for 1 year with varying sampling periodicities, and 16 PAHs were detected with concentrations ranging from 1 ng/PAS for chrysene to 9,727 ng/PAS for naphthalene. The PAS were found adapted to the monitoring of temporal and spatial variations for lightweight PAHs (up to four aromatic rings) though not for heavy PAHs with five aromatic rings or more, as these compounds are preferably in the particle phase of the atmosphere and the amount of these PAHs trapped on the PAS will be too low.

  2. Solid phase extraction for evaluation of occupational exposure to Pb (II) using XAD-4 sorbent prior to atomic absorption spectroscopy.

    PubMed

    Shahtaheri, Seyed Jamaleddin; Khadem, Monireh; Golbabaei, Farideh; Rahimi-Froushan, Abbas; Ganjali, Mohammad Reza; Norouzi, Parviz

    2007-01-01

    Lead is an important constituent widely used in different industrial processes. For evaluation of workers' exposure to trace toxic metal of Pb (II), solid-phase extraction (SPE) was optimized. SPE using mini columns filled with XAD-4 resin was developed with regard to sample pH, ligand concentration, loading flow rate, elution solvent, sample volume, elution volume, the amount of resins, and sample matrix interferences. Lead ions were retained on a solid sorbent and then eluted, followed by a simple determination of analytes with flame atomic absorption spectrometery. The obtained recoveries of metal ions were greater than 92%. This method was validated with 3 different pools of spiked urine samples; it showed a good reproducibility over 6 consecutive days as well as 6 within-day experiments. This optimized method can be considered successful in simplifying sample preparation for a trace residue analysis of lead in different matrices when evaluating occupational and environmental exposures is required.

  3. Chromatographic Separation of Glucose and Fructose

    NASA Astrophysics Data System (ADS)

    Kuptsevich, Yu E.; Larionov, Oleg G.; Stal'naya, I. D.; Nakhapetyan, L. A.; Pronin, A. Ya

    1987-03-01

    The structures, mutarotation, and the physicochemical properties of glucose and fructose as well as methods for their separation are examined. Their chromatographic separation on cation exchangers in the calcium-form is discussed in detail. A theory of the formation of complexes of carbohydrates with metal cations is described and the mechanism of the separation of glucose and fructose on cation exchangers in the calcium-form is discussed in detail. Factors influencing the chromatographic separation of glucose and fructose on sulphonic acid cation-exchange resins are also considered. The bibliography includes 138 references.

  4. Improvement of the fermentability of oxalic acid hydrolysates by detoxification using electrodialysis and adsorption.

    PubMed

    Jeong, So-Yeon; Trinh, Ly Thi Phi; Lee, Hong-Joo; Lee, Jae-Won

    2014-01-01

    A two-step detoxification process consisting of electrodialysis and adsorption was performed to improve the fermentability of oxalic acid hydrolysates. The constituents of the hydrolysate differed significantly between mixed hardwood and softwood. Acetic acid and furfural concentrations were high in the mixed hardwood, whereas 5-hydroxymethylfurfural (HMF) concentration was relatively low compared with that of the mixed softwood. The removal efficiency of acetic acid reached 100% by electrodialysis (ED) process in both hydrolysates, while those of furfural and HMF showed very low, due to non-ionizable properties. Most of the remaining inhibitors were removed by XAD-4 resin. In the mixed hardwood hydrolysate without removal of the inhibitors, ethanol fermentation was not completed. Meanwhile, both ED-treated hydrolysates successfully produced ethanol with 0.08 and 0.15 g/Lh ethanol productivity, respectively. The maximum ethanol productivity was attained after fermentation with 0.27 and 0.35 g/Lh of detoxified hydrolysates, which were treated by ED, followed by XAD-4 resin.

  5. Numerical Simulation of an Optical Chromatographic Separator

    DTIC Science & Technology

    2009-02-02

    its close relative, Bacillus thuringiensis ," Anal. Chem. 78, 3221-3225 (2006). 10. S. J. Hart, A. Terray, K. L. Kuhn, J. Arnold, and T. A. Leski...Terray, T. A. Leski, J. Arnold, and R. Stroud, "Discovery of a significant optical chromatographic difference between spores of Bacillus anthracis and

  6. 40 CFR 1065.267 - Gas chromatograph.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  7. 40 CFR 1065.267 - Gas chromatograph.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 33 2011-07-01 2011-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  8. Chromatographic methods in the study of autism.

    PubMed

    Żurawicz, Ewa; Kałużna-Czaplińska, Joanna; Rynkowski, Jacek

    2013-10-01

    Research into biomarkers of autism is a new means of medical intervention in this disease. Chromatographic techniques, especially coupled with mass spectrometry, are widely used in determination of biomarkers and assessment of effectiveness of autism therapy owing to their sensitivity and selectivity. Among the chromatographic techniques gas chromatography and liquid chromatography, especially high-performance liquid chromatography, have found application in clinical trials. The high-performance liquid chromatography technique allows an analysis of liquid samples with a wide range of molecules, small and large, providing an opportunity to perform advanced assays within a short time frame. Gas chromatography with the appropriate preparation of samples (gaseous and liquid) and a selection of analysis conditions enables the separation of thermally stable, volatile and non-volatile organic substances in short runtimes. The chromatographic techniques that are currently used in metabolic studies in autism are designed to identify abnormalities in three areas: the metabolism of neurotransmitters, nutritional and metabolic status and manifestations of oxidative stress. This review presents a necessary theoretical introduction and examples of applications of chromatographic studies of disorder markers in autism.

  9. Nano-fabricated size exclusion chromatograph

    NASA Technical Reports Server (NTRS)

    Svehla, D.; Feldman, S.; Feldman, J.; Grunthaner, F.; Shakkottai, P.; dle Castillo, L.; White, V.

    2002-01-01

    This poster describes the development of a nano-fabricated size exclusion chromatograph (nSEC) based on the principle that molecules traveling through a microcolumn containing nano-fabricated features will have characteristics elution times that directly correlate to molecular weight.

  10. Functional chromatographic technique for natural product isolation†

    PubMed Central

    Lau, Eric C.; Mason, Damian J.; Eichhorst, Nicole; Engelder, Pearce; Mesa, Celestina; Kithsiri Wijeratne, E. M.; Gunaherath, G. M. Kamal B.; Leslie Gunatilaka, A. A.

    2015-01-01

    Natural product discovery arises through a unique interplay between chromatographic purification and biological assays. Currently, most techniques used for natural product purification deliver leads without a defined biological action. We now describe a technique, referred to herein as functional chromatography, that deploys biological affinity as the matrix for compound isolation. PMID:25588099

  11. Method to fabricate silicon chromatographic column comprising fluid ports

    DOEpatents

    Manginell, Ronald P.; Frye-Mason, Gregory C.; Heller, Edwin J.; Adkins, Douglas R.

    2004-03-02

    A new method for fabricating a silicon chromatographic column comprising through-substrate fluid ports has been developed. This new method enables the fabrication of multi-layer interconnected stacks of silicon chromatographic columns.

  12. A Small-Scale Low-Cost Gas Chromatograph

    ERIC Educational Resources Information Center

    Gros, Natasa; Vrtacnik, Margareta

    2005-01-01

    The design and application of a small-scale portable gas chromatograph for learning of the basic concepts of chromatography is described. The apparatus consists of two basic separable units, which includes a chromatographic unit and an electronic unit.

  13. Method for the chromatographic separation of cations from aqueous samples

    DOEpatents

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

    1997-07-29

    An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methanediphosphonic acid on an inert particulate support. 7 figs.

  14. Enhanced adsorption of puerarin onto a novel hydrophilic and polar modified post-crosslinked resin from aqueous solution.

    PubMed

    Zeng, Xiaowei; Chen, Hongbo; Zheng, Yi; Tao, Wei; Fan, Yunge; Huang, Laiqiang; Mei, Lin

    2012-11-01

    A novel of hydrophilic and polar N-vinylpyrrolidone modified post-crosslinked resin was synthesized and the adsorption behaviors toward puerarin from aqueous solution were investigated. The post-crosslinked adsorbent PNVP-DVBpc was prepared by Friedel-Crafts reaction of residual double bonds without external crosslinking agent. The specific surface area of precursor PNVP-DVB increased obviously after post-crosslinking modification. The synthesized adsorbents were characterized by BET surface area, Fourier transform infrared (FTIR), and scanning electron microscopy (SEM). The adsorption behaviors of puerarin from aqueous solution onto precursor PNVP-DVB and post-crosslinked adsorbent PNVP-DVBpc were thoroughly researched. Commercial polymeric adsorbents Amberlite XAD-4 and AB-8 were chosen as the comparison. Among the four media, PNVP-DVBpc presented the largest adsorption capacity of puerarin, which resulted from the synergistic effect of high specific surface area and polar groups (amide groups) onto the adsorbent matrix. Experimental results showed that equilibrium isotherms could be fitted by Freundlich model and the kinetic data could be characterized by pseudo-second order model reasonably. Column adsorption experiments indicated that the puerarin could be completely desorbed by 4.0 BV industrial alcohol. Continuous column adsorption-regeneration cycles demonstrated the PNVP-DVBpc without any significant adsorption capacity loss during operation.

  15. Tadpole toxicity prediction using chromatographic systems.

    PubMed

    Fernández-Pumarega, Alejandro; Amézqueta, Susana; Fuguet, Elisabet; Rosés, Martí

    2015-10-30

    Toxicity has been emulated in tadpole species through chromatographic systems. The parameter studied to evaluate the non-specific toxicity of a compound is the narcosis concentration (Cnar), which is defined as the concentration needed for the immobilization of the organism. Because experimental investigation with animals is lengthy, costly, technically difficult, and ethically questionable, there is a great interest in developing surrogate physicochemical systems able to emulate biological systems to obtain the same information in a faster, more economic, and easier manner. In order to see which chromatographic systems would be able to emulate tadpole narcosis, both, tadpole narcosis data and data in several chromatographic and electrophoretic systems, were fitted to a linear solvation energy relationship (LSER) model. Thus, by comparison of the models it was possible to see which of the chromatographic systems were more similar to the biological one. The physicochemical systems that best emulate tadpole narcosis were an HPLC system based on an immobilized artificial membrane (IAM) column, and two micellar electrokinetic chromatography (MEKC) systems based on sodium taurocholate (STC) and a mixture of sodium dodecylsulphate (SDS) and Brij 35 as surfactants. A system based on a RP18 HPLC column also was selected for comparison because it is a common column in most analytical laboratories. To establish the models, a set of compounds with known Cnar values were analyzed in the chromatographic, and electrophoretic selected systems and, then, the retention factor (k) was correlated to the concentration of narcosis. Statistics showed that the system based on STC micelles was the best to emulate toxicity in tadpoles. The robustness and predictive ability of the developed models were validated.

  16. Modeling the uptake of neutral organic chemicals on XAD passive air samplers under variable temperatures, external wind speeds and ambient air concentrations (PAS-SIM).

    PubMed

    Armitage, James M; Hayward, Stephen J; Wania, Frank

    2013-01-01

    The main objective of this study was to evaluate the performance and demonstrate the utility of a fugacity-based model of XAD passive air samplers (XAD-PAS) designed to simulate the uptake of neutral organic chemicals under variable temperatures, external wind speeds and ambient air concentrations. The model (PAS-SIM) simulates the transport of the chemical across the air-side boundary layer and within the sampler medium, which is segmented into a user-defined number of thin layers. Model performance was evaluated using data for polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) from a field calibration study (i.e., active and XAD-PAS data) conducted in Egbert, Ontario, Canada. With some exceptions, modeled PAS uptake curves are in good agreement with the empirical PAS data. The results are highly encouraging, given the uncertainty in the active air sampler data used as input and other uncertainties related to model parametrization (e.g., sampler-air partition coefficients, the influence of wind speed on sampling rates). The study supports the further development and evaluation of the PAS-SIM model as a diagnostic (e.g., to aid interpretation of calibration studies and monitoring data) and prognostic (e.g., to inform design of future passive air sampling campaigns) tool.

  17. Adsorption-driven translocation of polymer chain into nanopores

    NASA Astrophysics Data System (ADS)

    Yang, Shuang; Neimark, Alexander V.

    2012-06-01

    The polymer translocation into nanopores is generally facilitated by external driving forces, such as electric or hydrodynamic fields, to compensate for entropic restrictions imposed by the confinement. We investigate the dynamics of translocation driven by polymer adsorption to the confining walls that is relevant to chromatographic separation of macromolecules. By using the self-consistent field theory, we study the passage of a chain trough a small opening from cis to trans compartments of spherical shape with adsorption potential applied in the trans compartment. The chain transfer is modeled as the Fokker-Plank diffusion along the free energy landscape of the translocation pass represented as a sum of the free energies of cis and trans parts of the chain tethered to the pore opening. We investigate how the chain length, the size of trans compartment, the magnitude of adsorption potential, and the extent of excluded volume interactions affect the translocation time and its distribution. Interplay of these factors brings about a variety of different translocation regimes. We show that excluded volume interactions within a certain range of adsorption potentials can cause a local minimum on the free energy landscape, which is absent for ideal chains. The adsorption potential always leads to the decrease of the free energy barrier, increasing the probability of successful translocation. However, the translocation time depends non-monotonically of the magnitude of adsorption potential. Our calculations predict the existence of the critical magnitude of adsorption potential, which separates favorable and unfavorable regimes of translocation.

  18. Preparation of macroporous methacrylate-based monoliths for chromatographic applications by the Reactive Gelation Process.

    PubMed

    Bechtle, M; Butté, A; Storti, G; Morbidelli, M

    2010-07-09

    Polymeric monoliths are a relatively new separation medium for chromatographic applications. The innovative approach to produce such monoliths, the Reactive Gelation Process, presented by Marti et al. [1] for polystyrene macroporous materials is applied to a methacrylate-based material. It is shown that it is possible to create a macroporous structure by Reactive Gelation also with this polymer even if the properties of the material are different. Besides the analysis of the material by SEM and BET, several chromatographic methods are used to analyze the material properties. The ISEC experiments showed a much smaller size exclusion effect than in conventional packed beds. The permeability of the material is comparable to a packed bed with 4.13 μm particles. The column efficiency is not changing for increasing flow rates. Because of the high efficiency of the material, shorter columns are needed and therefore the comparatively low permeability is compensated. The monolith also exhibits a significant adsorption capacity for hydrophobic interaction, which makes it suitable for chromatographic purification processes.

  19. Chromatographic fingerprint analysis of Pycnogenol dietary supplements.

    PubMed

    Chen, Pei; Song, Fenhong; Lin, Long-Ze

    2009-01-01

    The bark of maritime pine (Pinus pinaster Aiton) has been widely used as a remedy for various degenerative diseases. A standard high-performance liquid chromatographic (HPLC) procedure for Pycnogenol analysis is a method specified in the United States Pharmacopeia (USP) monograph, which requires measurement of peak areas and identification of four components of the extract: caffeic acid, catechin, ferulic acid, and taxifolin. In this study, a fingerprint analysis using an HPLC method based on the USP monograph has been developed to provide additional qualitative information for the analysis of Pycnogenol-containing dietary supplements (PDS). Twelve commercially available PDS samples were purchased and analyzed along with a standard Pycnogenol extract. Their chromatographic fingerprints were analyzed using principal component analysis. The results showed that two of the samples were not consistent with the standard reference Pycnogenol extract. One contained other active ingredients in addition to Pycnogenol, and the other may have resulted from a quality control issue in manufacturing.

  20. Micro-column plasma emission liquid chromatograph

    DOEpatents

    Gay, Don D.

    1984-01-01

    In a direct current plasma emission spectrometer for use in combination with a micro-column liquid chromatograph, an improved plasma source unit. The plasma source unit includes a quartz capillary tube having an inlet means, outlet off gas means and a pair of spaced electrodes defining a plasma region in the tube. The inlet means is connected to and adapted to receive eluant of the liquid chromatograph along with a stream of plasma-forming gas. There is an opening through the wall of the capillary tube penetrating into the plasma region. A soft glass capillary light pipe is disposed at the opening, is connected to the spectrometer, and is adapted to transmit light passing from the plasma region to the spectrometer. There is also a source of electromotive force connected to the electrodes sufficient to initiate and sustain a plasma in the plasma region of the tube.

  1. Chromatographic purification of highly active yeast ribosomes.

    PubMed

    Meskauskas, Arturas; Leshin, Jonathan A; Dinman, Jonathan D

    2011-10-24

    Eukaryotic ribosomes are much more labile as compared to their eubacterial and archael counterparts, thus posing a significant challenge to researchers. Particularly troublesome is the fact that lysis of cells releases a large number of proteases and nucleases which can degrade ribosomes. Thus, it is important to separate ribosomes from these enzymes as quickly as possible. Unfortunately, conventional differential ultracentrifugation methods leaves ribosomes exposed to these enzymes for unacceptably long periods of time, impacting their structural integrity and functionality. To address this problem, we utilize a chromatographic method using a cysteine charged Sulfolink resin. This simple and rapid application significantly reduces co-purifying proteolytic and nucleolytic activities, producing high yields of intact, highly biochemically active yeast ribosomes. We suggest that this method should also be applicable to mammalian ribosomes. The simplicity of the method, and the enhanced purity and activity of chromatographically purified ribosome represents a significant technical advancement for the study of eukaryotic ribosomes.

  2. Nano-fabricated size exclusion chromatograph

    NASA Technical Reports Server (NTRS)

    Svehla, D.; Feldman, S.; Feldman, J.; Grunthaner, F.; Shakkottai, P.; Castillo, L. del; White, V.

    2002-01-01

    This paper describes the development of a nano-fabricated size exclusion chromatograph (nSEC) based on the principle that molecules traveling through amicrocolumn containing nano-fabricated features will have characteristic elution times that directly correlate to molecular weight. Compared to conventional size exclusion chromatography, the nSEC offers greater control over the size exclusion process; mass fabrication; integration of the separation column with associated valves, pumps, and detectors; and dramatic reductions in instrument mass and power requirements.

  3. Use of a modified Tenax GC column packing for the direct gas chromatographic analysis of phenols in water at the ppm level.

    PubMed

    Bartle, K D; Elstub, J; Novotny, M; Robinson, R J

    1977-05-21

    Dilute solutions of phenols in water at the ppm level may be analysed gas chromatographically by direct injection onto a column with a packing similar to that used in the Viking 1975 spacecraft: Tenax GC (2,6-diphenyl-p-phenylene oxide polymer) modified with polymetaphenyl ether liquid phase to eradicate irreversible adsorption. Symmetrical peaks were observed for injections of less than 1 ng of phenol and some of its alkylated derivatives. Chromatographic properties of modified Tenax GC columns are reported along with their application to the analysis of some industrial effluents with previous work-up.

  4. A model free method for estimation of complicated adsorption isotherms in liquid chromatography.

    PubMed

    Forssén, Patrik; Fornstedt, Torgny

    2015-08-28

    Here we show that even extremely small variations in the adsorption isotherm can have a tremendous effect on the shape of the overloaded elution profiles and that the earlier in the adsorption isotherms the variation take place, the larger its impact on the shape of the elution profile. These variations are so small that they can be "hidden" by the discretization and in the general experimental noise when using traditional experimental methods, such as frontal analysis, to measure adsorption isotherms. But as the effects of these variations are more clearly visible in the elution profiles, the Inverse Method (IM) of adsorption isotherm estimation is an option. However, IM usually requires that one selects an adsorption isotherm model prior to the estimation process. Here we show that even complicated models might not be able to estimate the adsorption isotherms with multiple inflection points that small variations might give rise to. We therefore developed a modified IM that, instead of fixed adsorption isotherm models, uses monotone piecewise interpolation. We first validated the method with synthetic data and showed that it can be used to estimate an adsorption isotherm, which accurately predicts an extremely "strange" elution profile. For this case it was impossible to estimate the adsorption isotherm using IM with a fixed adsorption model. Finally, we will give an example of a real chromatographic system where adsorption isotherm with inflection points is estimated by the modified IM.

  5. Adsorption and desorption properties of macroporous resins for anthocyanins from the calyx extract of roselle (Hibiscus sabdariffa L.).

    PubMed

    Chang, Xiu-Lian; Wang, Dong; Chen, Bi-Yun; Feng, Yong-Mei; Wen, Shao-Hong; Zhan, Peng-Yuan

    2012-03-07

    Adsorption of roselle anthocynins, a natural pigment, onto various macroporous resins was optimized to develop a simple and efficient process for industrial separation and purification of roselle anthocyanins. Nine different macroporous resins (AB-8, X-5, HPD-100, SP-207, XAD-4, LS-305A, DM-21, LS-610B, and LS-305) were evaluated for the adsorption properties of the anthocyanins extracted from the calyx extract of Hibiscus sabdariffa L. The influences of phase contact time, solution pH, initial anthocyanin concentration, and ethanol concentration with different citric acid amounts were studied by the static adsorption/desorption method. The adsorption isotherm data were fitted well to the Langmuir isotherm, and according to this model, LS-610B and LS-305 exhibited the highest monolayer sorption capacities of 31.95 and 38.16 mg/g, respectively. The kinetic data were modeled using pseudo-first-order, pseudo-second-order, and intraparticle diffusion equations. The experimental data were well described by the pseudo-second-order kinetic model. Continuous column adsorption-regeneration cycles indicated negligible capacity loss of LS-305 during operation. The overall yield of pigment product was 49.6 mg/g dried calyces. The content of roselle anthocynins in the pigment product was 4.85%.

  6. [Optimization of two-dimensional high performance liquid chromatographic columns for highly efficient separation of intact proteins].

    PubMed

    Hong, Guangfeng; Gao, Mingxia; Yan, Guoquan; Guan, Xia; Tao, Qian; Zhang, Xiangmin

    2010-02-01

    In order to optimize two-dimensional liquid chromatographic (2D-LC) columns for highly efficient separation of proteins, several liquid chromatographic columns were investigated and evaluated. Weak anion-exchange (WAX) column was chosen as the first dimension because of its extensive protein separation power. By comparison of different WAX chromatographic columns for human liver protein separation, TSKgel DEAE-5PW column was selected as the first dimension of a 2D-LC system. For the second dimension, ten typical reversed-phase (RP) LC columns (250 mm x 4.6 mm, 5 microm, 30 nm) were investigated and evaluated. Their silica based RP stationary phases were butyl (C4), octyl (C8) or octadecyl (C18). To evaluate the retention behavior and non-specific protein adsorption ability of these ten columns, four neutral compounds (uracil, nitrobenzene, naphthalene and fluorene) and three standard proteins (cytochrome C, myoglobin and albumin from chicken egg white) were adopted and separated by RPLC. Meantime, WAX fractions were used to investigate the separation ability of different alkyl-bonded silica stationary phase columns for complex protein samples. By comparison of column separation efficiency, adsorption of intact proteins and sample analysis, Jupiter 300 C4 column was finally employed for its excellent separation ability. Optimization of WAX and RPLC columns offers reliable foundation for the construction of 2D-LC protein separation systems.

  7. Mesoscopic simulation of adsorption of peptides in a hydrophobic chromatography system.

    PubMed

    Makrodimitris, Kosta; Fernandez, Erik J; Woolf, Thomas B; O'Connell, John P

    2005-03-01

    Mesoscopic simulations using Langevin dipoles on a lattice for the solvent and calculated partial charges for the solute have been used to estimate free energies of adsorption from data on reversed-phase chromatography on nine protected peptides covering a wide range of structures. There is a single parameter, the effective solvent dipole moment, that is fit to data for one peptide and used to predict properties of the other eight peptides. Good agreement of adsorption chemical potentials, including order of chromatographic retention times, is found for calculations that are Boltzmann-averaged over a set of orientations. In addition, the results suggest that there are preferential orientations for each peptide at the model hydrophobic chromatographic surface. Estimation methods for adsorption based on molecular descriptors and hydrophobicity scales are shown to be unreliable for these systems. With refinements and extensions, this simulation method should be applicable to solvents containing salt, such as in hydrophobic interaction chromatography, and to larger solutes including proteins.

  8. Fractionation of Natural Organic Matter Upon Adsorption to the Bacterium, Bacillus subtilis

    NASA Astrophysics Data System (ADS)

    Manecki, M.; Maurice, P. A.; Fein, J. B.

    2001-12-01

    High pressure size exclusion chromatography (HPSEC) was used to measure changes in molecular weight distribution and average molecular weight upon adsorption of fulvic acid onto Bacillus subtilis at pH 3-7. The FA was an XAD-8 extract from a stream in the New Jersey Pine Barrens (USA), and had a weight average molecular weight of 1890 Da. Adsorption of aqueous FA onto B.subtilis was relatively fast, with steady state attained within 2 hours. An adsorption isotherm at pH 4.5 revealed a strong affinity of FA for the B.subtilis surface. The maximum adsorption capacity of a 20g bacteria/L suspension was greater than 9 mg C/L of FA at pH 4.5. Adsorption of FA onto B.subtilis was strongly pH dependent, increasing markedly with decreasing pH over the pH range 3-7. Comparison of HPSEC analysis of control (FA not reacted with bacteria) versus reacted samples showed that in all experiments, the weight average molecular weight (Mw) of FA remaining in solution decreased by several hundred Da. The observed decrease in solution Mw upon adsorption indicated that the higher molecular weight FA components adsorbed preferentially to the bacterial surfaces, at all studied pH values (3-7). Additionally, there was a low molecular weight FA fraction that did not adsorb, even at low pH. Our results suggest that hydrophobic interactions may be important for FA sorption to B.subtilis and that low molecular weight, more hydrophilic components may thus be less likely to adsorb than higher molecular weight, more hydrophobic components.

  9. PROBING REACTIVITY OF DISSOLVED ORGANIC MATTER FOR DISINFECTION BY-PRODUCT FORMATION USING XAD-8 RESIN ADSORPTION AND ULTRAFILTRATION FRACTIONATION. (R828045)

    EPA Science Inventory

    The disinfection by-product (DBP) reactivity (yield and speciation upon reaction with chlorine) of dissolved organic matter (DOM) isolated from two surface waters was investigated. The source waters, each having significantly different specific ultraviolet absorbance (SUVA

  10. High pressure liquid chromatographic gradient mixer

    DOEpatents

    Daughton, Christian G.; Sakaji, Richard H.

    1985-01-01

    A gradient mixer which effects the continuous mixing of any two miscible solvents without excessive decay or dispersion of the resultant isocratic effluent or of a linear or exponential gradient. The two solvents are fed under low or high pressure by means of two high performance liquid chromatographic pumps. The mixer comprises a series of ultra-low dead volume stainless steel tubes and low dead volume chambers. The two solvent streams impinge head-on at high fluxes. This initial nonhomogeneous mixture is then passed through a chamber packed with spirally-wound wires which cause turbulent mixing thereby homogenizing the mixture with minimum "band-broadening".

  11. Hand-held multiple system gas chromatograph

    DOEpatents

    Yu, Conrad M.

    2001-01-01

    A multiple parallel hand-held gas chromatograph (GC) system which includes several independent GCs. Each independent GC has its own injector, separation column, detector and oven and the GCs are mounted in a light weight hand-held assembly. Each GC operates independently and simultaneously. Because of different coatings in different separation columns, different retention times for the same gas will be measured. Thus, for a GC system with multiple parallel GCs, the system can measure, in a short period, different retention times and provide a cross-reference in the determination of the measured gas and to become a two-dimensional system for direct field use.

  12. High-pressure liquid chromatographic gradient mixer

    DOEpatents

    Daughton, C.G.; Sakaji, R.H.

    1982-09-08

    A gradient mixer effects the continuous mixing of any two miscible solvents without excessive decay or dispersion of the resultant isocratic effluent or of a linear or exponential gradient. The two solvents are fed under low or high pressure by means of two high performance liquid chromatographic pumps. The mixer comprises a series of ultra-low dead volume stainless steel tubes and low dead volume chambers. The two solvent streams impinge head-on at high fluxes. This initial nonhomogeneous mixture is then passed through a chamber packed with spirally-wound wires which cause turbulent mixing thereby homogenizing the mixture with minimum band-broadening.

  13. Packed multi-channels for parallel chromatographic separations in microchips.

    PubMed

    Nagy, Andrea; Gaspar, Attila

    2013-08-23

    Here we report on a simple method to fabricate microfluidic chip incorporating multi-channel systems packed by conventional chromatographic particles without the use of frits. The retaining effectivities of different bottlenecks created in the channels were studied. For the parallel multi-channel chromatographic separations several channel patterns were designed. The obtained multipackings were applied for parallel separations of dyes. The implementation of several chromatographic separation units in microscopic size makes possible faster and high throughput separations.

  14. Integrated immobilized cell reactor-adsorption system for beta-cyclodextrin production: a model study using PVA-cryogel entrapped Bacillus agaradhaerens cells.

    PubMed

    Martins, Rita F; Plieva, Fatima M; Santos, Ana; Hatti-Kaul, Rajni

    2003-09-01

    Production of cyclodextrins (CDs) by immobilized cells of the alkaliphilic Bacillus agaradhaerens LS-3C with integrated product recovery was studied. The microorganism was entrapped in polyvinyl alcohol-cryogel beads and used as a convenient source of immobilized cyclodextrin glycosyltransferase (CGTase). On activation by incubation in the cultivation medium containing 1% (w/v) starch, the entrapped cells multiplied and secreted CGTase with an activity of 2-3 mg beta-cyclodextrin h(-1) g(-1) beads. The immobilized biocatalyst exhibited maximum activity at pH 9 and 50 degrees C, and formed cyclodextrins comprising 92-94% beta-CD and remaining alpha-CD. The cyclodextrin product from the immobilized cell bioreactor was continuously recovered by adsorption to Amberlite XAD-4 in a recycle batch mode. The product adsorption was facilitated at low temperature while hot water was used for elution.

  15. [Contamination mechanism and regeneration strategies of chromatographic resin in separation process for expression product from mammary gland bioreactor].

    PubMed

    Sun, Xiyan; Zhang, Yan; Li, Yan; Luo, Jian; Qin, Peiyong; Su, Zhiguo

    2011-11-01

    This study focused on the contamination mechanism and regeneration strategies of sulfopropyl ion exchange resin (SP Sepharose FF) during the separation of recombinant human lactoferrin from transgenic bovine milk. We analyzed primary constituents' contents in chromatorgraphic material and fractions. The results showed that the lipid in milk can clog the column or adhere to the resin through hydrophobic interaction, leading to an increase in column pressure. Some casein molecules were found to adsorb onto the resin through electrostatic interaction, therefore the adsorption capacity was decreased. There was no direct interaction between lactose and the resin in the chromatorgraphic process. Increased continuous chromatographic cycles and prolonged time interval between protein purification and column regeneration could enhance the undesirable interaction between the contaminants and resin, thus lowering the regeneration efficiency. NaOH was found to be effective in the removal of lipid and casein molecules from the column. Furthermore, normal microstructure and chromatographic performance of the ion exchanger was recovered after this cleaning procedure.

  16. Versatile gas/particle ion chromatograph.

    PubMed

    Ullah, S M Rahmat; Takeuchi, Masaki; Dasgupta, Purnendu K

    2006-02-01

    A new, compact gas/particle ion chromatograph has been developed for measuring ionic constituents in PM2.5 (particulate matter of aerodynamic diameter < or = 2.5 microm) and water-soluble ionogenic gases. The instrument has separate sampling channels for gases and particles. In one, a membrane denuder collects soluble gases for preconcentration and analysis. In the other, a cyclone removes larger particles, a membrane denuder removes soluble gases, and a continuously wetted hydrophilic filter collects particles. A single, multiport, syringe pump handles liquid transport, and one conductivity detector measures anions and ammonium for both channels. Electrodialytically generated gradient hydroxide eluent permits 20 min chromatographic runs. Gas/particle samples are each collected for 40 min, butthe sampling intervals are staggered by 20 min. Liquid samples from the gas denuder and particle collector are aspirated and preconcentrated on sequential cation and anion concentrators and transferred respectively to an ammonia transfer device and an anion separation column. The flow configuration results in an ammonium peak before anion peaks in the chromatogram. The system measures ammonia, organic acids (such as acetic, formic, and oxalic acids), HCl, HONO, SO2, HNO3, and the corresponding ions in the aerosol phase. Low ng/m3 to sub-ng/m3 limits of detection (LODs) are attained for most common gases and particulate constituents, the LODs for gaseous SO2 to NH3 range, for example, from sub parts per trillion by volume (sub-pptv) to approximately 5 pptv.

  17. High performance hand-held gas chromatograph

    SciTech Connect

    Yu, C.M.

    1998-04-28

    The Microtechnology Center of Lawrence Livermore National Laboratory has developed a high performance hand-held, real time detection gas chromatograph (HHGC) by Micro-Electro-Mechanical-System (MEMS) technology. The total weight of this hand-held gas chromatograph is about five lbs., with a physical size of 8{close_quotes} x 5{close_quotes} x 3{close_quotes} including carrier gas and battery. It consumes about 12 watts of electrical power with a response time on the order of one to two minutes. This HHGC has an average effective theoretical plate of about 40k. Presently, its sensitivity is limited by its thermal sensitive detector at PPM. Like a conventional G.C., this HHGC consists mainly of three major components: (1) the sample injector, (2) the column, and (3) the detector with related electronics. The present HHGC injector is a modified version of the conventional injector. Its separation column is fabricated completely on silicon wafers by means of MEMS technology. This separation column has a circular cross section with a diameter of 100 pm. The detector developed for this hand-held GC is a thermal conductivity detector fabricated on a silicon nitride window by MEMS technology. A normal Wheatstone bridge is used. The signal is fed into a PC and displayed through LabView software.

  18. Adsorption Refrigeration System

    SciTech Connect

    Wang, Kai; Vineyard, Edward Allan

    2011-01-01

    Adsorption refrigeration is an environmentally friendly cooling technology which could be driven by recovered waste heat or low-grade heat such as solar energy. In comparison with absorption system, an adsorption system has no problems such as corrosion at high temperature and salt crystallization. In comparison with vapor compression refrigeration system, it has the advantages of simple control, no moving parts and less noise. This paper introduces the basic theory of adsorption cycle as well as the advanced adsorption cycles such as heat and mass recovery cycle, thermal wave cycle and convection thermal wave cycle. The types, characteristics, advantages and drawbacks of different adsorbents used in adsorption refrigeration systems are also summarized. This article will increase the awareness of this emerging cooling technology among the HVAC engineers and help them select appropriate adsorption systems in energy-efficient building design.

  19. BROAD SPECTRUM ANALYSIS FOR TRACE ORGANIC POLLUTANTS IN LARGE VOLUMES OF WATER BY XAD RESINS-COLUMN DESIGN-FACTS AND MYTHS.

    USGS Publications Warehouse

    Gibs, J.; Wicklund, A.; Suffet, I.H.

    1986-01-01

    The 'rule of thumb' that large volumes of water can be sampled for trace organic pollutants by XAD resin columns which are designed by small column laboratory studies or pure compounds is examined and shown to be a problem. A theory of multicomponent breakthrough is presented as a frame of reference to help solve the problem and develop useable criteria to aid the design of resin columns. An important part of the theory is the effect of humic substances on the breakthrough character of multicomponent chemical systems.

  20. Chromatographic behavior of the enantiomers of 2,2,2-trifluoro-1-(9-anthryl)ethanol on a quinidine-carbamate chiral stational phase

    SciTech Connect

    Asnin, Leonid; Gotmar, Gustaf; Guiochon, Georges A

    2005-08-01

    The enantioseparation of 2,2,2-trifluoro-1-(9-anthryl)ethanol on silica-bonded quinidine carbamate was examined under linear chromatographic conditions. The significant impact of nonselective adsorption on the retention was demonstrated. The influences of a polar additive in the mobile phase on the retention, the selectivity and the thermodynamic quantities of the retention were measured. A small effect of the pressure on the selectivity and on the accuracy of the thermodynamic measurements was observed.

  1. Fast gas chromatographic separation of biodiesel.

    SciTech Connect

    Pauls, R. E.

    2011-05-01

    A high-speed gas chromatographic method has been developed to determine the FAME distribution of B100 biodiesel. The capillary column used in this work has dimensions of 20 m x 0.100 mm and is coated with a polyethylene glycol film. Analysis times are typically on the order of 4-5 min depending upon the composition of the B100. The application of this method to a variety of vegetable and animal derived B100 is demonstrated. Quantitative results obtained with this method were in close agreement with those obtained by a more conventional approach on a 100 m column. The method, coupled with solid-phase extraction, was also found suitable to determine the B100 content of biodiesel-diesel blends.

  2. Detection system for a gas chromatograph

    DOEpatents

    Hayes, John M.; Small, Gerald J.

    1984-01-01

    A method and apparatus are described for the quantitative analysis of vaporizable compounds, and in particular of polycyclic aromatic hydrocarbons which may be induced to fluoresce. The sample to be analyzed is injected into a gas chromatography column and is eluted through a narrow orifice into a vacuum chamber. The free expansion of the eluted sample into the vacuum chamber creates a supersonic molecular beam in which the sample molecules are cooled to the extent that the excited vibrational and rotational levels are substantially depopulated. The cooled molecules, when induced to fluoresce by laser excitation, give greatly simplified spectra suitable for analytical purposes. The laser induced fluorimetry provides great selectivity, and the gas chromatograph provides quantitative transfer of the sample to the molecular beam.

  3. Liquid chromatographic determination of melamine in beverages.

    PubMed

    Ishiwata, H; Inoue, T; Yamazaki, T; Yoshihira, K

    1987-01-01

    A liquid chromatographic method is described for the determination of melamine in beverages. Melamine is separated by column chromatography using cation and anion exchange resin and determined by ion-pair liquid chromatography using an ODS column and a mixture of acetonitrile and 0.05M phosphate buffer (pH 3.0) containing 0.005M sodium 1-laurylsulfate (1 + 4, v/v) as mobile phase. Recoveries of melamine ranged between 90.3 +/- 7.8 and 102.1 +/- 5.6% at levels of 0.6 to 2.4 ppm in 4 kinds of beverages. The quantitation limit was 2.5 micrograms melamine in 50 mL beverage. The method was applied to the migration test of melamine from melamine-formaldehyde resin products to the beverages.

  4. Gas Chromatographic Detectors for Exobiology Flight Experiments

    NASA Technical Reports Server (NTRS)

    Kojiro, Daniel R.; Humphry, Donald E.; Takeuchi, Nori; Chang, Sherwood (Technical Monitor)

    1997-01-01

    Exobiology flight experiments require highly sensitive instrumentation for in situ chemical analysis of the volatile chemical species that occur in the atmospheres and surfaces of various bodies within the solar system. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. Future missions to Mars', comets, or planetary moons such as Europa, will perform experiments with complex analyses. In addition, instrumentation for such missions must perform under severely restricted conditions with limited resources. To meet these analytical requirements, improved methods and highly sensitive yet smaller instruments must continually be developed with increasingly greater capabilities. We describe here efforts to achieve this objective, for past and future missions, through the development of new or the improvement of existing sensitive, miniaturized gas chromatographic detectors.

  5. Interface for liquid chromatograph-mass spectrometer

    DOEpatents

    Andresen, B.D.; Fought, E.R.

    1989-09-19

    A moving belt interface is described for real-time, high-performance liquid chromatograph (HPLC)/mass spectrometer (MS) analysis which strips away the HPLC solvent as it emerges from the end of the HPLC column and leaves a residue suitable for mass-spectral analysis. The interface includes a portable, stand-alone apparatus having a plural stage vacuum station, a continuous ribbon or belt, a drive train magnetically coupled to an external drive motor, a calibrated HPLC delivery system, a heated probe tip and means located adjacent the probe tip for direct ionization of the residue on the belt. The interface is also capable of being readily adapted to fit any mass spectrometer. 8 figs.

  6. Interface for liquid chromatograph-mass spectrometer

    DOEpatents

    Andresen, Brian D.; Fought, Eric R.

    1989-01-01

    A moving belt interface for real-time, high-performance liquid chromatograph (HPLC)/mass spectrometer (MS) analysis which strips away the HPLC solvent as it emerges from the end of the HPLC column and leaves a residue suitable for mass-spectral analysis. The interface includes a portable, stand-alone apparatus having a plural stage vacuum station, a continuous ribbon or belt, a drive train magnetically coupled to an external drive motor, a calibrated HPLC delivery system, a heated probe tip and means located adjacent the probe tip for direct ionization of the residue on the belt. The interface is also capable of being readily adapted to fit any mass spectrometer.

  7. High-capacity pressurized continuous chromatograph

    SciTech Connect

    Begovich, J.M.; Byers, C.H.; Sisson, W.G.

    1983-01-01

    Multicomponent liquid chromatographic separations have been achieved by using a slowly rotating annular bed of sorbent material. The feed material is continuously introduced at a stationary point at the top of the bed, and eluent is allowed to flow everwhere else around the annulus. The rotation of the sorbent bed causes the separation components to appear as helical bands, each of which has a characteristic, stationary exit point; hence the separation process is truly continuous. The concept has been developed primarily on a 279-mm-diam by 0.6-m-long device with a 12.7-mm-wide annulus. The effects of annulus width and diameter have been studied using the same device with annulus widths up to 114.3 mm. With this largest width, approximately 96% of the area available within the outer cylinder is devoted to the rotating sorbent bed. Further annulus-width studies have been pursued on units with 89- and 445-mm diameters. These geometric extensions to the basic concept allow extremely large capacity increases with minimal loss in separation and no increase in chromatograph diameter. The effects associated with increased feed concentration have also been studied. In this effort as well as in the annulus-width program, the separation of copper, nickel, and cobalt components from a carbonate solution was studied in detail. The nickel and cobalt components are found in the leach liquor of the Caron process for recovering nickel and cobalt from laterite ores. Nominally 50-..mu..m0-diam Dowex 50W-X8 cation exchange resin was used as the bed material. The nickel concentration of the feed was varied tenfold, from 136.1 to approximately 1400 meq/L. The combined effects of the bed loading and annulus width were studied and compared with nonlinear theory.

  8. High-capacity pressurized continuous chromatograph

    SciTech Connect

    Begovich, J.M.; Byers, C.H.; Sisson, W.G.

    1983-01-01

    Multicomponent liquid chromatographic separations have been achieved by using a slowly rotating annular bed of sorbent material. The feed material is continuously introduced at a stationary point at the top of the bed, and eluent is allowed to flow everywhere else around the annulus. The rotation of the sorbent bed causes the separated components to appear as helical bands, each of which has a characteristic, stationary exit point; hence the separation process is truly continuous. The concept has been developed primarily on a 279-mm-diam by 0.6-m-long device with a 12.7-mm-wide annulus. The effects of annulus width and diameter have been studied using the same device with annulus widths up to 114.3 mm. With this largest width, approximately 96% of the area available within the outer cylinder is devoted to the rotating sorbent bed. Further annulus-width studies have been pursued on units with 89- and 445-mm diameters. These geometric extensions to the basic concept allow extremely large capacity increases with minimal loss in separation and no increase in chromatograph diameter. The effects associated with increased feed concentration have also been studied. In this effort as well as in the annulus-width program, the separation of copper, nickel, and cobalt components from a carbonate solution was studied in detail. The nickel and cobalt components are found in the leach liquor of the Caron process for recovering nickel and cobalt from laterite ores. Nominally 50-..mu..m-diam Dowex 50W-X8 cation exchange resin was used as the bed material. The nickel concentration of the feed was varied tenfold, from 136.1 to approximately 1400 meq/L. The combined effects of the bed loading and annulus width were studied and compared with nonlinear theory. 17 references, 9 figures, 1 table.

  9. High-capacity pressurized continuous chromatograph

    SciTech Connect

    Begovich, J.M.; Byers, C.H.; Sisson, W.G.

    1983-01-01

    Multicomponent liquid chromatographic separations have been achieved by using a slowly rotating annular bed of sorbent material. The feed material is continuously introduced at a stationary point at the top of the bed, and eluent is allowed to flow everywhere else around the annulus. The rotation of the sorbent bed causes the separated components to appear as helical bands, each of which has a characteristic, stationary exit point; hence the separation process is truly continuous. The concept has been developed primarily on a 279-mm-diam by 0.6m-long device with a 12.7-mm-wide annulus. The effects of annulus width and diameter have been studied using the same device with annulus widths up to 114.3 mm. With this largest width, approximately 96% of the area available within the outer cylinder is devoted to the rotating sorbent bed. Further annulus-width studies have been pursued on units with 89- and 445-mm diameters. These geometric extensions to the basic concept allow extremely large capacity increases with minimal loss in separation and no increase in chromatograph diameter. The effects associated with increased feed concentration have also been studied. In this effort as well as in the annulus-width program, the separation of copper, nickel, and cobalt components from a carbonate solution was studied in detail. The nickel and cobalt components are found in the leach liquor of the Caron process for recovering nickel and cobalt from laterite ores. Nominally 50-..mu..m-diam Dowex 50W-X8 cation exchange resin was used as the bed material. The nickel concentration of the feed was varied tenfold, from 136.1 to approximately 1400 meq/L. The combined effects of the bed loading and annulus width were studied and compared with nonlinear theory. 9 figures, 1 table.

  10. FTIR gas chromatographic analysis of perfumes

    NASA Astrophysics Data System (ADS)

    Diederich, H.; Stout, Phillip J.; Hill, Stephen L.; Krishnan, K.

    1992-03-01

    Perfumes, natural or synthetic, are complex mixtures consisting of numerous components. Gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques have been extensively utilized for the analysis of perfumes and essential oils. A limited number of perfume samples have also been analyzed by FT-IR gas chromatographic (GC-FTIR) techniques. Most of the latter studies have been performed using the conventional light pipe (LP) based GC-FTIR systems. In recent years, cold-trapping (in a matrix or neat) GC-FTIR systems have become available. The cold-trapping systems are capable of sub-nanogram sensitivities. In this paper, comparison data between the LP and the neat cold-trapping GC- FTIR systems is presented. The neat cold-trapping interface is known as Tracer. The results of GC-FTIR analysis of some commercial perfumes is also presented. For comparison of LP and Tracer GC-FTIR systems, a reference (synthetic) mixture containing 16 major and numerous minor constituents was used. The components of the mixture are the compounds commonly encountered in commercial perfumes. The GC-FTIR spectra of the reference mixture was obtained under identical chromatographic conditions from an LP and a Tracer system. A comparison of the two sets of data thus generated do indeed show the enhanced sensitivity level of the Tracer system. The comparison also shows that some of the major components detected by the Tracer system were absent from the LP data. Closer examination reveals that these compounds undergo thermal decomposition on contact with the hot gold surface that is part of the LP system. GC-FTIR data were obtained for three commercial perfume samples. The major components of these samples could easily be identified by spectra search against a digitized spectral library created using the Tracer data from the reference mixture.

  11. In situ and Ex situ adsorption and recovery of betalains from hairy root cultures of Beta vulgaris.

    PubMed

    Rudrappa, Thimmaraju; Neelwarne, Bhagyalakshmi; Aswathanarayana, Ravishankar G

    2004-01-01

    Various adsorbents were screened for in situ recovery of betalain pigments effluxed from hairy root cultures of red beet, Beta vulgaris. Alumina/silica (1:1) appeared ideal, showing in situ adsorption of 97% in a unit time of 30 min accounting for in situ recovery of 71.39% of the total betalaine effluxed. Other adsorbents such as Amberlite series (XAD-2 and -4), cyclodextrin, maltodextrin, dextrin white, and starches such as wheat starch and corn starch exhibited very poor in situ adsorption properties. Pretreatment of adsorbents with methanol significantly improved the adsorption capacities of some of the adsorbents, with a highest adsorption of 97.2% for alumina followed by alumina/silica (1:1) and higher adsorption by XAD-2 and -4. Complete in situ adsorption equilibrium was reached in 20 min for a solution containing 2.5 mg mL(-)(1) of betalain in adsorbents alumina, silica, and a mixture of alumina and silica. In situ betalain adsorption parameters for alumina/silica were determined using the Langmuir isotherm model where the adsorption capacity was found to be 0.174 mg g(-)(1) and the adsorption energy was 0.9 at pH 5.5 and 25 degrees C. Desorption of pigments from the adsorbents was invariably highest in poor adsorbents, indicating their poor adsorption energy for betalaines. Similarly, recovery by desorption was low in those adsorbents having high adsorption capacity, indicating that adsorbents such as activated ones with highest adsorption capacity with zero desorption property were unsuitable for the recovery of effluxed pigments. Ex situ recovery of betalain done using various combinations of alumina/silica and processed sand and different column geometries indicated that alumina with processed sand at a 2:1 ratio (w/w) and a minimum column material of 2 cm height and 2 cm diameter was good enough to cause 97% pigment adsorption from a solution containing 1.6 mg mL(-)(1). Desorption and recovery of pigments ex situ from columns were affected by various

  12. A Simple Adsorption Experiment

    ERIC Educational Resources Information Center

    Guirado, Gonzalo; Ayllon, Jose A.

    2011-01-01

    The study of adsorption phenomenon is one of the most relevant and traditional physical chemistry experiments performed by chemistry undergraduate students in laboratory courses. In this article, we describe an easy, inexpensive, and straightforward way to experimentally determine adsorption isotherms using pieces of filter paper as the adsorbent…

  13. Analytical solutions and moment analysis of chromatographic models for rectangular pulse injections.

    PubMed

    Qamar, Shamsul; Abbasi, Javeria N; Javeed, Shumaila; Shah, Munawar; Khan, Farman U; Seidel-Morgenstern, Andreas

    2013-11-08

    This work focuses on the analysis of two standard liquid chromatographic models, namely the lumped kinetic model and the equilibrium dispersive model. Analytical solutions, obtained by means of Laplace transformation, are derived for rectangular single solute concentration pulses of finite length and breakthrough curves injected under linear conditions. In order to analyze the solute transport behavior by means of the two models, the temporal moments up to fourth order are calculated from the Laplace-transformed solutions. The limiting cases of continuous injection and negligible mass transfer limitations are evaluated. For validation, the analytical solutions are compared with the numerical solutions of models using the discontinuous Galerkin finite element method. Results of different case studies are discussed for linear and nonlinear adsorption isotherms. The discontinuous Galerkin method is employed to obtain moments for both linear and nonlinear models numerically. Analytically and numerically determined concentration profiles and moments were found to be in good agreement.

  14. Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4.

    PubMed

    Kara, Derya; Fisher, Andrew; Hill, Steve J

    2009-06-15

    A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1M HNO(3) directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

  15. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) coupled to XAD fractionation: Method to algal organic matter characterization.

    PubMed

    Nicolau, Rudy; Leloup, Maud; Lachassagne, Delphine; Pinault, Emilie; Feuillade-Cathalifaud, Geneviève

    2015-05-01

    This work is focused on the development of an analytical procedure for the improvement of the Organic Matter structure characterization, particularly the algal matter. Two fractions of algal organic matter from laboratory cultures of algae (Euglena gracilis) and cyanobacteria (Microcystis aeruginosa) were extracted with XAD resins. The fractions were studied using laser desorption ionization (LDI) and Matrix-Assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF). A comparison with the natural organic matter characteristics from commercial humic acids and fulvic acids extracted from Suwannee River was performed. Results show that algal and natural organic matters have unique quasi-polymeric structures. Significant repeating patterns were identified. Different fractions extracted from organic matter with common origin had common structures. Thus, 44, 114 and 169Da peaks separation for fractions from E. gracilis organic matter and 28, 58 and 100Da for M. aeruginosa ones were clearly observed. Using the developed protocol, a structural scheme and organic matter composition were obtained. The range 600-2000Da contained more architectural composition differences than the range 100-600Da, suggesting that organic matter is composed of an assembly of common small molecules. Associated to specific monomers, particular patterns were common to all samples but assembly and resulting structure were unique for each organic matter. Thus, XAD fractionation coupled to mass spectroscopy allowed determining a specific fingerprint for each organic matter.

  16. Numerical estimation of adsorption energy distributions from adsorption isotherm data with the expectation-maximization method

    SciTech Connect

    Stanley, B.J.; Guiochon, G. |

    1993-08-01

    The expectation-maximization (EM) method of parameter estimation is used to calculate adsorption energy distributions of molecular probes from their adsorption isotherms. EM does not require prior knowledge of the distribution function or the isotherm, requires no smoothing of the isotherm data, and converges with high stability towards the maximum-likelihood estimate. The method is therefore robust and accurate at high iteration numbers. The EM algorithm is tested with simulated energy distributions corresponding to unimodal Gaussian, bimodal Gaussian, Poisson distributions, and the distributions resulting from Misra isotherms. Theoretical isotherms are generated from these distributions using the Langmuir model, and then chromatographic band profiles are computed using the ideal model of chromatography. Noise is then introduced in the theoretical band profiles comparable to those observed experimentally. The isotherm is then calculated using the elution-by-characteristic points method. The energy distribution given by the EM method is compared to the original one. Results are contrasted to those obtained with the House and Jaycock algorithm HILDA, and shown to be superior in terms of robustness, accuracy, and information theory. The effect of undersampling of the high-pressure/low-energy region of the adsorption is reported and discussed for the EM algorithm, as well as the effect of signal-to-noise ratio on the degree of heterogeneity that may be estimated experimentally.

  17. Rapid process development of chromatographic process using direct analysis in real time mass spectrometry as a process analytical technology tool.

    PubMed

    Yan, Binjun; Chen, Teng; Xu, Zhilin; Qu, Haibin

    2014-06-01

    The concept of quality by design (QbD) is widely applied in the process development of pharmaceuticals. However, the additional cost and time have caused some resistance about QbD implementation. To show a possible solution, this work proposed a rapid process development method, which used direct analysis in real time mass spectrometry (DART-MS) as a process analytical technology (PAT) tool for studying the chromatographic process of Ginkgo biloba L., as an example. The breakthrough curves were fast determined by DART-MS at-line. A high correlation coefficient of 0.9520 was found between the concentrations of ginkgolide A determined by DART-MS and HPLC. Based on the PAT tool, the impacts of process parameters on the adsorption capacity were discovered rapidly, which showed a decreased adsorption capacity with the increase of the flow rate. This work has shown the feasibility and advantages of integrating PAT into QbD implementation for rapid process development.

  18. Chromatographic and traditional albumin isotherms on cellulose: a model for wound protein adsorption on modified cotton

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Albumin is the most abundant protein found in healing wounds. Traditional and chromatogrpahic protein isotherms of albumin binding on modified cotton fibers are useful in understanding albumin binding to cellulose wound dressings. An important consideration in the design of cellulosic wound dressin...

  19. Adsorption behavior of alpha -cypermethrin on cork and activated carbon.

    PubMed

    Domingues, Valentina F; Priolo, Giuseppe; Alves, Arminda C; Cabral, Miguel F; Delerue-Matos, Cristina

    2007-08-01

    Studies were undertaken to determine the adsorption behavior of alpha -cypermethrin [R)-alpha -cyano-3-phenoxybenzyl(1S)-cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate, and (S)-alpha-cyano-3-phenoxybenzyl (1R)-cis-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropanecarboxylate] in solutions on granules of cork and activated carbon (GAC). The adsorption studies were carried out using a batch equilibrium technique. A gas chromatograph with an electron capture detector (GC-ECD) was used to analyze alpha -cypermethrin after solid phase extraction with C18 disks. Physical properties including real density, pore volume, surface area and pore diameter of cork were evaluated by mercury porosimetry. Characterization of cork particles showed variations thereby indicating the highly heterogeneous structure of the material. The average surface area of cork particles was lower than that of GAC. Kinetics adsorption studies allowed the determination of the equilibrium time - 24 hours for both cork (1-2 mm and 3-4 mm) and GAC. For the studied alpha -cypermethrin concentration range, GAC revealed to be a better sorbent. However, adsorption parameters for equilibrium concentrations, obtained through the Langmuir and Freundlich models, showed that granulated cork 1-2 mm have the maximum amount of adsorbed alpha-cypermethrin (q(m)) (303 microg/g); followed by GAC (186 microg/g) and cork 3-4 mm (136 microg/g). The standard deviation (SD) values, demonstrate that Freundlich model better describes the alpha -cypermethrin adsorption phenomena on GAC, while alpha -cypermethrin adsorption on cork (1-2 mm and 3-4 mm) is better described by the Langmuir. In view of the adsorption results obtained in this study it appears that granulated cork may be a better and a cheaper alternative to GAC for removing alpha -cypermethrin from water.

  20. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    SciTech Connect

    Liu, Ying

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  1. Adsorption and removal kinetics of phosphonate from water using natural adsorbents.

    PubMed

    Kumar, R Anil; Velayudhan, K T; Ramachandran, V; Bhai, R Susheela; Unnikrishnan, G; Vasu, K

    2010-01-01

    The removal of phosphonate from water was studied using some natural adsorbents. Potassium phosphonate is a fungicide used for the control of Phytophthora capsici, which is prevalent in black pepper (Piper nigrum L.). Batch adsorption kinetic experiments were conducted on the adsorption of phosphonate onto the adsorbents. The concentration of phosphonate was measured on a high-performance liquid chromatograph fitted with a conductivity detector. The percentage removal of phosphonate by powdered laterite stone (PLS) from water was 40.4%, within a residence time of 15 minutes. The mechanisms of the rate of adsorption were analyzed and compared using the pseudo-second-order, Elovich, and intraparticle diffusion models. The experimental data was found to correlate well with the pseudo-second-order kinetic model, indicating adsorption as a chemisorption process. A possible reaction in the phosphonate-PLS system also has been proposed. The PLS can be used as a low-cost natural adsorbent for phosphonate removal from water.

  2. Studies on improved integrated membrane-based chromatographic process for bioseparation

    NASA Astrophysics Data System (ADS)

    Xu, Yanke

    To improve protein separation and purification directly from a fermentation broth, a novel membrane filtration-cum-chromatography device configuration having a relatively impermeable coated zone near the hollow fiber module outlet has been developed. The integrated membrane filtration-cum-chromatography unit packed with chromatographic beads on the shell side of the hollow fiber unit enjoys the advantages of both membrane filtration and chromatography; it allows one to load the chromatographic media directly from the fermentation broth or lysate and separate the adsorbed proteins through the subsequent elution step in a cyclic process. Interfacial polymerization was carried out to coat the bottom section of the hollow fiber membrane while leaving the rest of the hollow fiber membrane unaffected. Myoglobin (Mb), bovine serum albumin (BSA) and a-lactalbumin (a-LA) were used as model proteins in binary mixtures. Separation behaviors of binary protein mixtures were studied in devices using either an ultrafiltration (UF) membrane or a microfiltration (MF) membrane. Experimental results show that the breakthrough time and the protein loading capacities were dramatically improved after coating in both UF and MF modules. For a synthetic yeast fermentation broth feed, the Mb and a-LA elution profiles for the four consecutive cyclic runs were almost superimposable. Due to the lower transmembrane flux in this device plus the periodical washing-elution during the chromatographic separation, fouling was not a problem as it is in conventional microfiltration. A mathematical model describing the hydrodynamic and protein loading behaviors of the integrated device using UF membrane with a coated zone was developed. The simulation results for the breakthrough agree well with the experimental breakthrough curves. The optimal length of the coated zone was obtained from the simulation. A theoretical analysis of the protein mass transfer was performed using a diffusion-convection model

  3. Tailing of chromatographic peaks in GC-MS caused by interaction of halogenated solvents with the ion source.

    PubMed

    Brocks, Jochen J; Hope, Janet M

    2014-07-01

    The injection of analytes into a gas chromatography-mass spectrometry (GC-MS) system using dichloromethane (DCM) as solvent led to gradual deterioration of chromatographic signals, with significant tailing and loss of sensitivity for C17+ hydrocarbons. The injector, gas chromatograph and transfer line were excluded as causes. Normal peak shape could only be restored by the insertion of a cleaned MS ion source. To elucidate potential surficial contaminants, the ion source was heated from 260 to 320°C, leading to the release of increasing concentrations of ferrous chloride [FeCl2(g)]. The ferrous chloride probably formed through the decomposition of DCM on metal surfaces in the ion source. We posit that the tailing was caused by the adsorption of analytes to sub-µm layers of FeCl2 at crystal defect sites in the metal, followed by the slow release of molecules back into the gas phase. There are at least two other cases in the literature in which tailing is specifically associated with the use of halogenated solvents. However, it is possible that the problem is relatively common, albeit rarely diagnosed and reported. The tailing of chromatographic peaks caused by the formation of ferrous chloride in the mass spectrometer can be diagnosed by scanning the MS background signal for the diagnostic isotopic pattern of FeCl2(+). The problem is easily solved by cleaning the MS ion source and avoiding halogenated solvents.

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

    SciTech Connect

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

    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 and 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)

  5. Chromatographic Separation of Vitamin E Enantiomers.

    PubMed

    Fu, Ju-Yen; Htar, Thet-Thet; De Silva, Leanne; Tan, Doryn Meam-Yee; Chuah, Lay-Hong

    2017-02-04

    Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  6. [Combination similarity algorithm on chromatographic fingerprints].

    PubMed

    Zhan, Xueyan; Shi, Xinyuan; Duan, Tianxuan; Li, Lei; Qiao, Yanjiang

    2010-11-01

    The similarity of chromatographic fingerprints is one of the effective approaches evaluating the quality stability of Chinese medicine, and the cosine of angle plays an important role in the application of similarity. However, the cosine approach is insensitive to the data difference when the distribution range of the data sets is wide. When the data proportion of the reference sample and the test sample is greatly different, it confirms that the sensitivity of the cosine to the differences of the peaks owned by both the reference sample and the test sample differs from the peaks owned only by the reference sample or the test sample in this study. The method considers the peaks owned by one sample in addition to peaks owned by both samples, and determines their own appropriate weigh targeting for the maximal homostasis value of proportion among the peaks of all of Smilax glabra Roxb. samples. The method based on sample data could reflect the difference in the chemical composition area ratio between the reference sample and test samples sensitively, and measures the similarity among the nine Smilax glabra Roxb. samples, which is a new similarity algorithm for evaluating the quality stability of herbal medicines.

  7. Hybrid adsorptive membrane reactor

    NASA Technical Reports Server (NTRS)

    Tsotsis, Theodore T. (Inventor); Sahimi, Muhammad (Inventor); Fayyaz-Najafi, Babak (Inventor); Harale, Aadesh (Inventor); Park, Byoung-Gi (Inventor); Liu, Paul K. T. (Inventor)

    2011-01-01

    A hybrid adsorbent-membrane reactor in which the chemical reaction, membrane separation, and product adsorption are coupled. Also disclosed are a dual-reactor apparatus and a process using the reactor or the apparatus.

  8. Generalized random sequential adsorption

    NASA Astrophysics Data System (ADS)

    Tarjus, G.; Schaaf, P.; Talbot, J.

    1990-12-01

    Adsorption of hard spherical particles onto a flat uniform surface is analyzed by using generalized random sequential adsorption (RSA) models. These models are defined by releasing the condition of immobility present in the usual RSA rules to allow for desorption or surface diffusion. Contrary to the simple RSA case, generalized RSA processes are no longer irreversible and the system formed by the adsorbed particles on the surface may reach an equilibrium state. We show by using a distribution function approach that the kinetics of such processes can be described by means of an exact infinite hierarchy of equations reminiscent of the Kirkwood-Salsburg hierarchy for systems at equilibrium. We illustrate the way in which the systems produced by adsorption/desorption and by adsorption/diffusion evolve between the two limits represented by ``simple RSA'' and ``equilibrium'' by considering approximate solutions in terms of truncated density expansions.

  9. Hybrid adsorptive membrane reactor

    SciTech Connect

    Tsotsis, Theodore T.; Sahimi, Muhammad; Fayyaz-Najafi, Babak; Harale, Aadesh; Park, Byoung-Gi; Liu, Paul K. T.

    2011-03-01

    A hybrid adsorbent-membrane reactor in which the chemical reaction, membrane separation, and product adsorption are coupled. Also disclosed are a dual-reactor apparatus and a process using the reactor or the apparatus.

  10. CHROMATOGRAPHIC AND MASS SPECTRAL STUDIES OF PERFLUOROOCTANESULFONATE AND THREE PERFLUOROOCTANESULFONAMIDES

    EPA Science Inventory

    The chromatographic and mass spectral characteristics of perfluorooctanesulfonate (PFOS) and three nitrogen-substituted perfluorooctanesulfonamides have been obtained. A methyl/phenol mixed phase fused silica capillary column was used for GC analysis, while a C18 reversed phase ...

  11. Efficient wheat germ agglutinin purification with a chitosan-based affinity chromatographic matrix.

    PubMed

    Baieli, María F; Urtasun, Nicolás; Miranda, María V; Cascone, Osvaldo; Wolman, Federico J

    2012-01-01

    An efficient affinity chromatographic matrix based on chitosan for wheat germ agglutinin (WGA) purification was developed. The matrices assayed consisted of chitosan mini-spheres cross-linked with epichlorhydrin 45, 250 or 500 mM. The maximum adsorption capacity of pure WGA - calculated from the corresponding isotherms - was between 43.2 and 48.9 mg/g at pH 5.0 and between 16.6 and 27.6 mg/g at pH 8.5. However, the adsorption of agglutinin from wheat germ extract was higher at pH 8.5. In addition, 0.5 g of mini-spheres cross-linked with epichlorhydrin 250 mM adsorbed 94.5% of the WGA present in 5 mL of the concentrated extract. Acetic acid was able to elute 100% of the adsorbed WGA. The purity of the WGA obtained was greater than 95% and the purification factor was 56.8. The matrix was able to maintain an efficient performance of the purification process for three consecutive cycles. A new method to monitor the purification process by RP-HPLC was developed.

  12. Gas chromatographic separation of hydrogen isotopes using metal hydrides

    SciTech Connect

    Aldridge, F.T.

    1984-05-09

    A study was made of the properties of metal hydrides which may be suitable for use in chromatographic separation of hydrogen isotopes. Sixty-five alloys were measured, with the best having a hydrogen-deuterium separation factor of 1.35 at 60/sup 0/C. Chromatographic columns using these alloys produced deuterium enrichments of up to 3.6 in a single pass, using natural abundance hydrogen as starting material. 25 references, 16 figures, 4 tables.

  13. Method for liquid chromatographic extraction of strontium from acid solutions

    DOEpatents

    Horwitz, E. Philip; Dietz, Mark L.

    1992-01-01

    A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

  14. Quantifying process tradeoffs in the operation of chromatographic sequences.

    PubMed

    Ngiam, Sheau-Huey; Bracewell, Daniel G; Zhou, Yuhong; Titchener-Hooker, Nigel J

    2003-01-01

    A method for the rapid representation of key process tradeoffs that need to be made during the analysis of chromatographic sequences has been proposed. It involves the construction of fractionation and maximum purification factor versus yield diagrams, which can be completed easily on the basis of chromatographic data. The output of the framework developed reflects the degree of tradeoff between levels of yield and purity and provides a fast and precise prediction of the sample fraction collection strategy needed to meet a desired process specification. The usefulness of this approach for the purposes of product purification and contaminant removal in a single chromatographic step has been successfully demonstrated in an earlier paper and it is now extended by application to a chromatographic sequence: the separation of a hypothetical three-component protein system by hydrophobic interaction chromatography (HIC) followed by size exclusion chromatography (SEC). The HIC operation has a strong impact upon the subsequent SEC step. The studies show how the analysis of performance in such a chromatographic sequence can be carried out easily and in a straightforward fashion using the fractionation diagram approach. The methodology proposed serves as a useful tool for identifying the process tradeoffs that must be made during operation of a sequence of chromatographic steps and indicates the impact on further processing of the cut-point decisions that are made.

  15. Use of expanded bed adsorption to purify flavonoids from Ginkgo biloba L.

    PubMed

    Li, Jing; Chase, Howard A

    2009-12-11

    Three techniques (liquid-liquid extraction, packed bed adsorption and expanded bed adsorption) have been compared for the purification of flavonoids from the leaves of Ginkgo biloba L. A crude Ginkgo extract was obtained by refluxing with ethanol for 3h. The yield of flavonoids achieved by this crude extraction was about 19% (w/w) and the purity of flavonoids in the concentrated extract was between 1.9 and 2.3% (w/w). The crude extract was then dissolved in deionized water and centrifuged where necessary to prepare clarified feedstock for further purification. For the method using liquid-liquid extraction with ethyl acetate, the purity, concentration ratio and yield of flavonoids were 25.4-31.0%, 16-18 and >98%, respectively. For the method using packed bed adsorption, Amberlite XAD7HP was selected as the adsorbent and clarified extract was used as the feedstock. The dynamic adsorption breakthrough curves and elution profiles were measured. For a feedstock containing flavonoids at a concentration of 0.25mg/mL, the appropriate loading volume to reach a 5% breakthrough point during the adsorption stage was estimated to be 550-600 mL for a packed bed of volume 53 mL and a flow rate of 183 cm/h. The results from the elution stage indicated that the majority of impurities were eluted by ethanol concentrations of 40% (v/v) or below and efficient separation of flavonoids from the impurities could be achieved by elution of the flavonoids with 50-80% ethanol reaching an average purity of approximately 25%. The recovery yield of flavonoids using the packed bed purification method was about 60% of the flavonoids present in the clarified feedstock (corresponding to around 30% for the total flavonoids in the unclarified crude extract). For the method using expanded bed adsorption also conducted with Amberlite XAD7HP as the adsorbent, the optimal operation conditions scouted during the packed bed experiments were used but unclarified crude extract could be loaded directly into

  16. Simultaneous preconcentration of Co(II), Ni(II), Cu(II), and Cd(II) from environmental samples on Amberlite XAD-2000 column and determination by FAAS.

    PubMed

    Duran, Celal; Senturk, Hasan Basri; Elci, Latif; Soylak, Mustafa; Tufekci, Mehmet

    2009-02-15

    A new method for the preconcentration of some trace metals (Co, Ni, Cu, and Cd) as complexed with ammonium pyrrolidynedithiocarbamate (APDC) was developed using a mini-column filled with Amberlite XAD-2000 resin. Metal contents were determined by flame atomic absorption spectrometry (FAAS) after the metal complexes accumulated on the resin were eluted with 1M HNO(3) in acetone. The effects of the analytical parameters such as sample pH, quantity of complexing agent, eluent type, resin quantity, sample volume, sample flow rate, and matrix ions were investigated on the recovery of the metals from aqueous solutions. The relative standard deviation (R.S.D.) of the method was <6%. The validation of the method was confirmed using two certified reference materials (CRM TMDW-500 Drinking Water and CRM SA-C Sandy Soil C). The method was successfully applied to some stream waters and mushroom samples from Eastern Black Sea Region (Trabzon city) of Turkey.

  17. Protein adsorption in polyelectrolyte brush type cation-exchangers.

    PubMed

    Khalaf, Rushd; Coquebert de Neuville, Bertrand; Morbidelli, Massimo

    2016-11-04

    Ion exchange chromatography materials functionalized with polyelectrolyte brushes (PEB) are becoming an integral part of many protein purification steps. Adsorption onto these materials is different than that onto traditional materials, due to the 3D partitioning of proteins into the polyelectrolyte brushes. Despite this mechanistic difference, many works have described the chromatographic behavior of proteins on polyelectrolyte brush type ion exchangers with much of the same methods as used for traditional materials. In this work, unconventional chromatographic behavior on polyelectrolyte brush type materials is observed for several proteins: the peaks shapes reveal first anti-Langmuirian and then Langmuirian types of interactions, with increasing injection volumes. An experimental and model based description of these materials is carried out in order to explain this behavior. The reason for this behavior is shown to be the 3D partitioning of proteins into the polyelectrolyte brushes: proteins that fully and readily utilize the 3D structure of the PEB phase during adsorption show this behavior, whereas those that do not show traditional ion exchange behavior.

  18. Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent for preconcentrations of Cd2+ and Co2+ and their determination by ICP-OES.

    PubMed

    Özdemir, Sadin; Okumuş, Veysi; Kılınç, Ersin; Bilgetekin, Havin; Dündar, Abdurrahman; Ziyadanogˇulları, Berrin

    2012-09-15

    This article reports a method that is used for the preconcentration and determination of Cd(2+) and Co(2+) in vegetables, using Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent. The concentrations of metals were determined by inductively coupled plasma-optical spectrometry (ICP-OES). Critical parameters, such as the pH of the solution, flow rate, the amount of biosorbent, type and volume of eluent, and the sample volume, that affect the solid-phase extraction (SPE) procedure were optimized. The optimum extraction conditions were determined as being a pH of 6.0 for Cd(2+) and of 5.0 for Co(2+); a sample flow rate of 2.0 mL min(-1); 200.0mg of biosorbent; and 5.0 mL of 1.0 mol L(-1) HCl as eluent. The capacities of the biosorbent for metal uptake were found to be 11.3 and 9.8 mg g(-1) for Cd(2+) and Co(2+) ions, respectively. Limit of quantitations (LOQs) were found to be 0.67 and 0.82 ng mL(-1), respectively, for Cd(2+) and Co(2+). The linear working curves were observed to be in the linear range from 1.0 to 50.0 ng mL(-1), and possessed high correlation coefficients. The use of the SPE method showed 50.7- and 35.7-fold improvements in the sensitivities of ICP-OES. The developed method was successfully applied to NCS ZC-73014 (a certified reference tea sample). Relative standard deviations (RSD) were lower than 5.0%. The Cd(2+) and Co(2+) concentrations in the different parts (leave, root, stem, and fruit) of purslane, onion, rocket, okra, and aubergine were determined after microwave digestion and solid-phase extraction by P. eryngii immobilized on Amberlite XAD-16.

  19. Comparison of polyurethane foam and XAD-2 sampling matrices to measure airborne organophosphorus pesticides and their oxygen analogs in an agricultural community.

    PubMed

    Armstrong, Jenna L; Fenske, Richard A; Yost, Michael G; Tchong-French, Maria; Yu, Jianbo

    2013-07-01

    Side-by-side active air sampling for the organophosphorus (OP) pesticide, chlorpyrifos (CPF) and its oxygen analog, chlorpyrifos-oxon (CPF-O) was conducted with two recommended air sampling matrices: OSHA Versatile Sampling (OVS) tubes with XAD-2 resin, polyurethane foam (PUF) tubes, and passive PUF deposition disks. The study compared the proportion of artificially transformed CPF-O in the laboratory and in the field during a tree fruit application in Washington State. Lab results demonstrated that the NIOSH-recommended OVS tubes artificially transformed up to 32% of CPF to CPF-O during the sampling process, whereas PUF tubes had little to no artificial transformation (⩽0.1%). In the field, the proportion of CPF-O in the sample was significantly higher on OVS tubes than on PUF tubes (p<0.001), confirming that OVS tubes were converting a significant portion of CPF to CPF-O. In addition, PUF tubes reported measurable levels CPF-O in the field even when no artificial transformation was expected. We conclude that the PUF matrix is the superior sampling medium for OP oxygen analogs when compared to XAD-two resin. Community-located PUF tube samples 24h post-application had considerably higher levels CPF-O (16-21ngm(-3)) than near field samples during application (2-14ngm(-3)), suggesting that the oxygen analog is volatile and formed during atmospheric transport. It is recommended that worker and community risk assessments begin to take into consideration the presence of the more toxic oxygen analogs when measuring for OP pesticide mixtures.

  20. Adsorption of star polymers

    NASA Astrophysics Data System (ADS)

    Halperin, A.; Joanny, J. F.

    1991-06-01

    The adsorption of star polymers on a flat solid surface is analyzed by means of scalling arguments based on the Daoud-Cotton blob model. For the adsorption of a single star, consisting of f arms comprising each N monomers, we distinguish three regimes determined by the adsorption energy of a monomer at the surface, δ kT. 1) Strong adsorption characterized by the full adsorption of all arms occurs for δ > (f/N)^{3/5}. 2) A “Sombrero” like structure comprising f_ads fully adsorbed arms and f{-}f_ads free arms is obtained for (f/N)^{3/5}> δ > f^{9/20}/N^{3/5}. 3) Weakly adsorbed stars retain, essentially, the structure of a free star. This regime occurs for δ < f^{9/20}/N^{3/5}. The weakly adsorbed structure may also exist as a metastable state if δ > f^{9/5}/N^{3/5}. Nous étudions l'adsorption de polymères en étoile sur une surface solide en utilisant une approche de lois d'échelles basée sur le modèle de blobs de Daoud et Cotton. Pour une étoile formée de f bras contenant chacun N monomères, nous distinguons trois régimes suivant la valeur de l'énergie d'adsorption d'un monomère sur la surface δ kT. 1) L'adsorption forte caractérisée par une adsorption complète de tous les bras se produit lorsque δ > (f/N)^{3/5}. 2) Une structure en “sombrero” avec f_ads bras adsorbés et f{-}f_ads bras libres est obtenue si f^{9/20}/N^{3/5}δ < (f/N)^{3/5}. 3) Les étoiles faiblement adsorbées gardent une structure très similaire à celle des étoiles libres en solution. Ce régime existe si δ < f^{9/20}/N^{3/5}. La structure correspondant aux étoiles faiblement adsorbées peut aussi exister comme un état métastable si δ > f^{9/5}/N^{3/5}.

  1. Laser temperature jump relaxation measurements of adsorption/desorption kinetics at liquid/solid interfaces

    SciTech Connect

    Waite, S.W.; Harris, J.M.; Holzwarth, J.F.

    1995-04-15

    The iodine laser temperature jump method is used to study adsorption/desorption kinetics at a methylated silica/solution interface. A suspension of C1-derivatized fumed silica is used for the kinetic measurements. The colloidal silica does not significantly change the attenuation of near-IR radiation from the iodine laser and allows the surface site concentration to be varied so that adsorption and desorption rates can be determined. The temperature jump relaxation method was used to investigate the effect of electrolyte on adsorption of a charged solute (ANS) on a C1 silica surface. Adsorption equilibrium conditions were optimized to observe a maximum relaxation signal. Without electrolyte, the relaxation signal is biexponential, which is also reflected in a broad chromatographic peak shape and a two-site sorption isotherm. When electrolyte is added, the relaxation signal is primarily single exponential, which agrees with the linear adsorption isotherm. The adsorption rate and equilibrium constant were found to increase significantly with added electrolyte, which showed that adsorption kinetics can influence both band broadening and retention. 28 refs., 7 figs., 4 tab.

  2. Recovery of polyphenols from rose oil distillation wastewater using adsorption resins--a pilot study.

    PubMed

    Rusanov, Krasimir; Garo, Eliane; Rusanova, Mila; Fertig, Orlando; Hamburger, Matthias; Atanassov, Ivan; Butterweck, Veronika

    2014-11-01

    The production of rose oil from rose flowers by water steam distillation leaves a water fraction of the distillate as main part of the waste. Therefore, the rose oil distillation wastewater represents a serious environmental problem due to the high content of polyphenols which are difficult to decompose and have to be considered as biopollutants when discarded into the drainage system and rivers. On the other hand, natural polyphenols are valuable compounds with useful properties as bioactive substances. Until now there is no established practice for processing of rose oil distillation wastewater and utilization of contained substances. Thus, it was the aim of this study to develop a strategy to separate this wastewater into a polyphenol depleted water fraction and a polyphenol enriched fraction which could be developed into innovative value-added products. In a first step, the phytochemical profile of rose oil distillation wastewater was determined. Its HPLC-PDA-MS analysis revealed the presence of flavan-3-ols, flavanones, flavonols and flavones. In a second step, the development of a stepwise concentration of rose oil distillation wastewater was performed. The concentration process includes a filtration process to eliminate suspended solids in the wastewater, followed by adsorption of the contained phenolic compounds onto adsorption resins (XAD and SP). Finally, desorption of the polyphenol fraction from the resin matrix was achieved using ethanol and/or aqueous ethanol. The result of the process was a wastewater low in soluble organic compounds and an enriched polyphenol fraction (RF20 SP-207). The profile of this fraction was similar to that of rose oil distillation wastewater and showed the presence of flavonols such as quercetin and kaempferol glycosides as major metabolites. These compounds were isolated from the enriched polyphenol fraction and their structures confirmed by NMR. In summary, a pilot medium scale system was developed using adsorption resins

  3. New Adsorption Methods.

    ERIC Educational Resources Information Center

    Wankat, Phillip C.

    1984-01-01

    Discusses a simple method for following the movement of a solute in an adsorption or ion exchange system. This movement is used to study a variety of operational methods, including continuous flow and pulsed flow counter-current operations and simulated counter-current systems. Effect of changing thermodynamic variables is also considered. (JM)

  4. SEPARATION BY ADSORPTION

    DOEpatents

    Lowe, C.S.

    1959-06-16

    Separation of Pu from fission products by adsorption on hydrous aluminum silicate is described. The Pu in a HNO/sub 3/ solution is oxidized to the hexavalent state and contacted with the silicate which adsorbs fission products. (T.R.H.)

  5. Continuous melting and ion chromatographic analyses of ice cores.

    PubMed

    Huber, T M; Schwikowski, M; Gäggele, H W

    2001-06-22

    A new method for determining concentrations of organic and inorganic ions in ice cores by continuous melting and contemporaneous ion chromatographic analyses was developed. A subcore is melted on a melting device and the meltwater produced is collected in two parallel sample loops and then analyzed simultaneously by two ion chromatographs, one for anions and one for cations. For most of the analyzed species, lower or equal blank values were achieved with the continuous melting and analysis technique compared to the conventional analysis. Comparison of the continuous melting and ion chromatographic analysis with the conventional analysis of a real ice core segment showed good agreement in concentration profiles and total amounts of ionic species. Thus, the newly developed method is well suited for ice core analysis and has the advantages of lower ice consumption, less time-consuming sample preparation and lower risk of contamination.

  6. Ion-exchange chromatographic analysis of peroxynitric acid.

    PubMed

    Nakashima, Yoichi; Ikawa, Satoshi; Tani, Atsushi; Kitano, Katsuhisa

    2016-01-29

    Ion-exchange chromatographic analysis of peroxynitric acid (O2NOOH) was performed by combining an acidic eluate with an UV-vis detector and immersing the separation column in an ice-water bath. The decomposition behavior of peroxynitric acid in the solution was also studied using this system. The fraction for the peroxynitric acid peak was collected. Ion-exchange chromatographic analysis of this fraction, after standing at room temperature for 24h, showed that the decomposition products were mainly nitrate ions with a very small amount of nitrous acid. The peroxynitric acid peak area correlated perfectly with the total amount of decomposition products. The ion-exchange chromatographic isolation allowed us to evaluate the molar extinction coefficient of peroxynitric acid precisely in a wider wavelength range than previous reports. The value decreases monotonically from 1729±26M(-1)cm(-1) at 200nm to 12.0±0.5M(-1)cm(-1) at 290nm.

  7. Mathematical functions for the representation of chromatographic peaks.

    PubMed

    Di Marco, V B; Bombi, G G

    2001-10-05

    About ninety empirical functions for the representation of chromatographic peaks have been collected and tabulated. The table, based on almost 200 references, reports for every function: (1) the most used name; (2) the most convenient equation, with the existence intervals for the adjustable parameters and for the independent variable; (3) the applications; (4) the mathematical properties, in relation to the possible applications. The list includes also equations originally proposed to represent peaks obtained in other analytical techniques (e.g. in spectroscopy), which in many instances have proved useful in representing chromatographic peaks as well; the built-in functions employed in some commercial peak-fitting software packages were included, too. Some of the most important chromatographic functions, i.e. the Exponentially Modified Gaussian, the Poisson, the Log-normal, the Edgeworth/Cramér series and the Gram/Charlier series, have been reviewed and commented in more detail.

  8. [Derivative gas chromatographic analysis of fructooligosaccharide in fermented sucrose].

    PubMed

    Cai, W M; Liu, H; Sun, X J

    2000-01-01

    As a new sweetener, fructooligosaccharide is paid more and more attention for its health improvement property. It includes trisaccharide, tetrasaccharide and pentasaccharide, and can be produced from sucrose by the fermentation of microorganism. In order to analyze the content of fructooligosaccharide in fermented sugar by gas chromatography, fructooligosaccharide was transformed into trimethylsilyl derivatives. Based on the modified gas chromatograph SP2308, and under the chosen chromatographic conditions with 0.53 mm capillary column of OV-101, the contents of fructose, glucose, sucrose and fructooligosaccharide were determined by programmed temperature chromatography. The recovery of fructooligosaccharide was satisfactory.

  9. On-line gas chromatographic analysis of airborne particles

    DOEpatents

    Hering, Susanne V [Berkeley, CA; Goldstein, Allen H [Orinda, CA

    2012-01-03

    A method and apparatus for the in-situ, chemical analysis of an aerosol. The method may include the steps of: collecting an aerosol; thermally desorbing the aerosol into a carrier gas to provide desorbed aerosol material; transporting the desorbed aerosol material onto the head of a gas chromatography column; analyzing the aerosol material using a gas chromatograph, and quantizing the aerosol material as it evolves from the gas chromatography column. The apparatus includes a collection and thermal desorption cell, a gas chromatograph including a gas chromatography column, heated transport lines coupling the cell and the column; and a quantization detector for aerosol material evolving from the gas chromatography column.

  10. On the optimization of the solid core radius of superficially porous particles for finite adsorption rate.

    PubMed

    Kaczmarski, Krzysztof

    2011-02-18

    Packed chromatographic columns with the superficially porous particles (porous shell particles) guarantee higher efficiency. The theoretical equation of the Height Equivalent to a Theoretical Plate (HETP), for columns packed with spherical superficially porous particles, was used for the analysis of the column efficiency for finite rate of adsorption-desorption process. The HETP equation was calculated by the application of the moment analysis to elution peaks evaluated with the General Rate (GR) model. The optimal solid core radius for maximum column efficiency was estimated for a wide spectrum of internal and external mass transfer resistances, adsorption kinetic rate and axial dispersion. The separation power of the shell adsorbent for two component mixture, in analytical and preparative chromatography, was discussed. The conditions of the equivalence between the solutions of the General Rate model with slow adsorption kinetic and the Lumped Kinetic Model (LKM) or the Equilibrium Dispersive (ED) model were formulated.

  11. Binary and ternary adsorption of n-alkane mixtures on activated carbon

    SciTech Connect

    Kalies, G.; Braeuer, P.; Messow, U.

    1999-06-15

    The adsorption isotherms of the binary n-alkane mixtures n-hexane/n-octane, n-octane/n-tetradecane, and n-hexane/n-tetradecane on the activated carbon TA 95 are measured at 298 K and described with mathematical functions. About 40 experimental values of the adsorption excess of the ternary mixture n-hexane/n-octane/n-tetradecane on activated carbon TA 95 at 298 K are gas chromatographically measured inside the ternary triangle. The ternary data are represented in the three-dimensional space with the help of transformation of coordinates and by utilization of the conception of the quasi-two-component representation of the mole fractions. A consistency test for the specific wetting Gibbs energies calculated from the binary data is carried out. The possibilities for a mathematical prediction of ternary data from adsorption data for the constituent binary mixtures are proved.

  12. Separation of phenolic compounds with modified adsorption resin from aqueous phase products of hydrothermal liquefaction of rice straw.

    PubMed

    Chen, Kaifei; Lyu, Hang; Hao, Shilai; Luo, Gang; Zhang, Shicheng; Chen, Jianmin

    2015-04-01

    Hydrothermal liquefaction can be used to convert rice straw into an aqueous phase product that contains valuable phenolic compounds. In experiments, commercial adsorption resin XAD-4 was modified by a benzene ring - α,α'-dichloro-p-xylene (DCX) - in order to separate the phenolic compounds from the aqueous phase product; and, the optimal conditions for separation were explored. The results showed that, after modification of the resin, its adsorption capacity improved by 50%, due to increases in surface area, pore volume and micropore volume. The selectivity of the resin increased when the benzene ring was introduced as the ring formed hydrogen bonds with the compounds. The optimal conditions for separation were desorption agent of 40%, 45% and 55% ethanol solution, a flow rate of 2.5-5 mL/min, and a ratio of the sample volume to the column volume was 1:1. The total content of phenolic compounds in aqueous solution increased from 18% to 78% after separation.

  13. Chromatographic fingerprints analysis for evaluation of Ginkgo Biloba products

    Technology Transfer Automated Retrieval System (TEKTRAN)

    The leaf extract of Ginkgo biloba has purported value for improving mental capacities in Alzheimer’s patients. The flavonoids and the terpene lactones are considered to be the two main active components that influence human health. This paper compared an LC/UV chromatographic fingerprint method wi...

  14. On the ion chromatographic determination of S(IV)

    NASA Astrophysics Data System (ADS)

    Dasgupta, Purnendu K.

    Ion Chromatographie determination of S(IV) is described with special reference to the determination of SO 2(g) and/or aerosol S(IV) along with chloride, nitrate and sulfate in particulate matter. A method is presented for the baseline separation of the above species. The Chromatographic behavior of hydroxymethanesulfonate under various eluent conditions is discussed.

  15. [The gas chromatographic detection of acetylene in cadaveric material].

    PubMed

    Iablochkin, V D

    1999-01-01

    Acetylene traces were detected by gas chromatography in the cadaveric right crural muscle of a 30-year-old man dead from an explosion of an acetylene reservoir at a plant. Acetylene was identified using the absolute calibration method on 3 standard gas chromatographic columns, reaction gas chromatography, and acetylene "deduction" by silver sulfate on silicagel.

  16. Chromatographic profiles of Ginkgo biloba leaves and selected products

    Technology Transfer Automated Retrieval System (TEKTRAN)

    An LC-DAD-ESI/MS method was developed to obtain chromatographic profiles for the flavonoids and terpene lactones of Ginkgo biloba leaves and selected G. biloba products. The method was used to identify 46 glycosylated flavonols and flavones, 3 free flavonol aglycones, catechin, 10 biflavones, a dihy...

  17. Note on the chromatographic analyses of marine polyunsaturated fatty acids

    USGS Publications Warehouse

    Schultz, D.M.; Quinn, J.G.

    1977-01-01

    Gas-liquid chromatography was used to study the effects of saponification/methylation and thin-layer chromatographic isolation on the analyses of polyunsaturated fatty acids. Using selected procedures, the qualitative and quantitative distribution of these acids in marine organisms can be determined with a high degree of accuracy. ?? 1977 Springer-Verlag.

  18. Performance of chromatographic systems to model soil-water sorption.

    PubMed

    Hidalgo-Rodríguez, Marta; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

    2012-08-24

    A systematic approach for evaluating the goodness of chromatographic systems to model the sorption of neutral organic compounds by soil from water is presented in this work. It is based on the examination of the three sources of error that determine the overall variance obtained when soil-water partition coefficients are correlated against chromatographic retention factors: the variance of the soil-water sorption data, the variance of the chromatographic data, and the variance attributed to the dissimilarity between the two systems. These contributions of variance are easily predicted through the characterization of the systems by the solvation parameter model. According to this method, several chromatographic systems besides the reference octanol-water partition system have been selected to test their performance in the emulation of soil-water sorption. The results from the experimental correlations agree with the predicted variances. The high-performance liquid chromatography system based on an immobilized artificial membrane and the micellar electrokinetic chromatography systems of sodium dodecylsulfate and sodium taurocholate provide the most precise correlation models. They have shown to predict well soil-water sorption coefficients of several tested herbicides. Octanol-water partitions and high-performance liquid chromatography measurements using C18 columns are less suited for the estimation of soil-water partition coefficients.

  19. Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

    ERIC Educational Resources Information Center

    Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

    2008-01-01

    Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

  20. Regenerable adsorption system

    NASA Technical Reports Server (NTRS)

    Roychoudhury, Subir (Inventor); Perry, Jay (Inventor); Walsh, Dennis (Inventor)

    2006-01-01

    A method for regenerable adsorption includes providing a substrate that defines at least one layer of ultra short channel length mesh capable of conducting an electrical current therethrough, coating at least a portion of the substrate with a desired sorbent for trace contaminant control or CO.sub.2 sorption, resistively heating the substrate, and passing a flowstream through the substrate and in contact with the sorbent.

  1. Control of ice chromatographic retention mechanism by changing temperature and dopant concentration.

    PubMed

    Tasaki, Yuiko; Okada, Tetsuo

    2011-12-15

    A liquid phase coexists with solid water ice in a typical binary system, such as NaCl-water, in the temperature range between the freezing point and the eutectic point (t(eu)) of the system. In ice chromatography with salt-doped ice as the stationary phase, both solid and liquid phase can contribute to solute retention in different fashions; that is, the solid ice surface acts as an adsorbent, while a solute can be partitioned into the liquid phase. Thus, both adsorption and partition mechanisms can be utilized for ice chromatographic separation. An important feature in this approach is that the liquid phase volume can be varied by changing the temperature and the concentration of a salt incorporated into the ice stationary phase. Thus, we can control the relative contribution from the partition mechanism in the entire retention because the liquid phase volume can be estimated from the freezing depression curve. Separation selectivity can thereby be modified. The applicability of this concept has been confirmed for the solutes of different adsorption and partition abilities. The predicted retention based on thermodynamics basically agrees well with the corresponding experimental retention. However, one important inconsistency has been found. The calculation predicts a step-like discontinuity of the solute retention at t(eu) because the phase diagram suggests that the liquid phase abruptly appears at t(eu) when the temperature increases. In contrast, the corresponding experimental plots are continuous over the wider range including the subeutectic temperatures. This discrepancy is explained by the existence of the liquid phase below t(eu). A difference between predicted and measured retention factors allows the estimation of the volume of the subeutectic liquid phase.

  2. Diffusion Influenced Adsorption Kinetics.

    PubMed

    Miura, Toshiaki; Seki, Kazuhiko

    2015-08-27

    When the kinetics of adsorption is influenced by the diffusive flow of solutes, the solute concentration at the surface is influenced by the surface coverage of solutes, which is given by the Langmuir-Hinshelwood adsorption equation. The diffusion equation with the boundary condition given by the Langmuir-Hinshelwood adsorption equation leads to the nonlinear integro-differential equation for the surface coverage. In this paper, we solved the nonlinear integro-differential equation using the Grünwald-Letnikov formula developed to solve fractional kinetics. Guided by the numerical results, analytical expressions for the upper and lower bounds of the exact numerical results were obtained. The upper and lower bounds were close to the exact numerical results in the diffusion- and reaction-controlled limits, respectively. We examined the validity of the two simple analytical expressions obtained in the diffusion-controlled limit. The results were generalized to include the effect of dispersive diffusion. We also investigated the effect of molecular rearrangement of anisotropic molecules on surface coverage.

  3. An automated multidimensional preparative gas chromatographic system for isolation and enrichment of trace amounts of xenon from ambient air.

    PubMed

    Larson, Tuula; Östman, Conny; Colmsjö, Anders

    2011-04-01

    The monitoring of radioactive xenon isotopes is one of the principal methods for the detection of nuclear explosions in order to identify clandestine nuclear testing. In this work, a miniaturized, multiple-oven, six-column, preparative gas chromatograph was constructed in order to isolate trace quantities of radioactive xenon isotopes from ambient air, utilizing nitrogen as the carrier gas. The multidimensional chromatograph comprised preparative stainless steel columns packed with molecular sieves, activated carbon, and synthetic carbon adsorbents (e.g., Anasorb®-747 and Carbosphere®). A combination of purification techniques--ambient adsorption, thermal desorption, back-flushing, thermal focusing, and heart cutting--was selectively optimized to produce a well-defined xenon peak that facilitated reproducible heart cutting and accurate quantification. The chromatographic purification of a sample requires approximately 4 h and provides complete separation of xenon from potentially interfering components (such as water vapor, methane, carbon dioxide, and radon) with recovery and accuracy close to 100%. The preparative enrichment process isolates and concentrates a highly purified xenon gas fraction that is suitable for subsequent ultra-low-level γ-, ß/γ-spectroscopic or high-resolution mass spectrometric measurement (e.g., to monitor the gaseous fission products of nuclear explosions at remote locations). The Xenon Processing Unit is a free-standing, relatively lightweight, and transportable system that can be interfaced to a variety of sampling and detection systems. It has a relatively inexpensive, rugged, and compact modular (19-inch rack) design that provides easy access to all parts for maintenance and has a low power requirement.

  4. The adsorption of hetero- and alicyclic thiophene derivatives from water-acetonitrile solutions on the surface of porous graphitic carbon under high-performance liquid chromatography conditions

    NASA Astrophysics Data System (ADS)

    Saifutdinov, B. R.; Emel'yanova, N. S.; Kurbatova, S. V.; Pimerzin, A. A.

    2012-07-01

    The adsorption of hetero- and alicyclic thiophene derivatives synthesized for the first time from water-acetonitrile solutions with various compositions on the surface of porous graphitic carbon was studied by the high-performance liquid chromatography method. The retention factor and Henry adsorption constant values and equilibrium constants of quasi-chemical reactions of the adsorption and solvation of the heterocyclic compounds studied were calculated using the Lanin-Nikitin equation. The influence of the structure of hetero- and alicyclic thiophene derivative molecules on their adsorption on the surface of porous graphitic carbon and solvation in water-acetonitrile solutions was discussed. The Lanin-Nikitin model was found to be more informative in the interpretation of the adsorption-chromatographic experiment data compared with the Snyder-Soczewinski and Scott-Kucera models.

  5. Chromatographic separation of platinum group metals from simulated high level liquid waste using macroporous silica-based adsorbents.

    PubMed

    Xu, Yuanlai; Kim, Seong-Yun; Ito, Tatsuya; Tokuda, Haruki; Hitomi, Keitaro; Ishii, Keizo

    2013-10-18

    To separate platinum group metals (PGMs) from high level liquid waste, three novel macroporous silica-based adsorbents, namely, (Crea+Dodec)/SiO2-P, (Crea+TOA)/SiO2-P and (MOTDGA+TOA)/SiO2-P, were synthesized by introducing extractants Crea (N',N'-di-n-hexyl-thiodiglycolamide), TOA (Tri-n-octylamine), MOTDGA (N,N'-dimethyl-N,N'-di-n-octyl-thiodiglycolamide) along with theirs modifier, Dodec (n-dodecyl alcohol), into 50μm diameter SiO2-P particles by impregnation. Chromatographic separation of PGMs from simulated high level liquid waste was investigated by column method. It was found that 100% of Pd(II) and Re(VII) could be eluted out from simulate HLLW in 3.0M HNO3 solution using three adsorbents. For Ru(III) and Rh(III), high temperature has distinct effect on the adsorption rate and a further study for Ru(III) and Rh(III) is necessary to separate them from HLLW completely. In all six column experiments, a relatively satisfactory chromatographic separation operating for PGMs from simulated HLLW was obtained using (Crea+TOA)/SiO2-P adsorbent packed column at 323K.

  6. Mutagenic potentials of Amberlite XAD-2-resin extracts obtained from river and drinking waters in the Northwest district of Chiba, Japan.

    PubMed

    Kanno, Ayako; Nishi, Iwaki; Kishi, Tomohiro; Kawakami, Tsuyoshi; Takahashi, Yasuo; Onodera, Sukeo

    2010-12-01

    Amberlite XAD-2 resin extracts of river and drinking water sampled from the Northwest district of Chiba Prefecture in each month during the period from January to December 2008 were investigated to characterize and determine their mutagenic potentials and polycyclic aromatic hydrocarbon (PAH) levels. The extracts from the river water were shown to be mutagenic in Salmonella typhimurium TA98 (a flameshift mutagen) without S9 mix, with higher mutagenic responses in summer and early fall seasons. While the drinking water extracts exhibited weak mutagenicity in both the TA98 and TA100 strains (a base-pair substitution mutagen) without S9 mix, with high mutagenic responses in fall and early winter seasons. GC/MS determinations of the water concentrates showed some seasonal scatter in PAH levels in river water. In contrast, comparatively high concentrations of PAHs were observed for drinking water samples collected during warmer seasons. Statistical studies revealed that there is a lower correlation between the levels of flameshift mutagenicity and the concentrations of PAH in the river water concentrations, but a higher correlation between them in the drinking water samples.

  7. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Chromatographic separation material for clinical... Laboratory Instruments § 862.2230 Chromatographic separation material for clinical use. (a) Identification. A chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents,...

  8. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Chromatographic separation material for clinical... Laboratory Instruments § 862.2230 Chromatographic separation material for clinical use. (a) Identification. A chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents,...

  9. Chromatographic behaviour of synthetic high pressure high temperature diamond in aqueous normal phase chromatography.

    PubMed

    Peristyy, Anton; Paull, Brett; Nesterenko, Pavel N

    2016-10-28

    The chromatographic properties of high pressure high temperature synthesised diamond (HPHT) are investigated under the conditions of hydrophilic interaction liquid chromatography (HILIC). A 50×4.6mm ID stainless steel column packed with HPHT particles of mean diameter 1.6μm and specific surface area 5.1m(2)g(-1) is used. According to the results of acid-base titration with NaOH the purified HPHT batch contains 4.59μeqg(-1) of protogenic, mainly carboxyl- and hydroxyl-, groups, which make this polar adsorbent suitable for use as a stationary phase in HILIC. The retention behaviour of several classes of polar compounds including benzoic and benzenesulfonic acids, nitro- and chlorophenols, various organic bases, and quaternary ammonium compounds are studied using acetonitrile and methanol based mobile phases containing 5-30v/v% of water. The effects of the buffer pH and concentration, column temperature and organic solvent content on retention of model compounds are also investigated. It is shown that both pH and acetonitrile/methanol ratio in the mobile phase can be used to vary the separation selectivity. Molecular adsorption mechanism (related to aqueous normal phase mode), rather than partitioning is established to be responsible for the retention.

  10. Loading capacity and chromatographic behavior of a porous graphitic carbon column for polychlorinated biphenyls

    USGS Publications Warehouse

    Echols, K.R.; Gale, R.W.; Feltz, K.; O'Laughlin, J.; Tillitt, D.E.; Schwartz, T.R.

    1998-01-01

    A porous graphitic carbon column (Hypercarb) was used for the fractionation of polychlorinated biphenyls (PCBs) into classes of 2-4 ortho chlorines, 1 ortho chlorine and 0 ortho chlorine congeners. A method was developed that combined the fractionation of PCBs, polychlorinated dibenzo- p-dioxins and dibenzofurans in a variety of biotic environmental samples. Many of these samples have high concentrations of PCBs which cause fractionation problems as adsorption sites on the graphitic surface are occupied. The loading capacity of the column for PCBs was determined by injecting up to 1 mg of total PCBs and monitoring changes in chromatographic behavior of tetra-/di-ortho, mono-ortho and non-ortho substituted PCBs. Effective loading capacities were 1 mg for tetra-/di-ortho PCBs, but only 3- 5 ??g for non-ortho PCBs and about 2 ??g for mono-ortho PCBs. Loading capacity of the PGC column for environmental fish and avian egg samples was determined to depend on the mono-ortho and non-ortho PCB levels found in these samples.

  11. Purge and trap with monolithic sorbent for gas chromatographic analysis of pesticides in honey.

    PubMed

    Chienthavorn, Orapin; Dararuang, Kanittha; Sasook, Anupop; Ramnut, Narumol

    2012-01-01

    Polydivinylbenzene (P-DVB) and silica monolithic materials were synthesised in capillaries and then used to adsorb nine organonitrogen pesticides extracted from honey. After adsorption, each monolith-capillary was connected to a gas chromatograph (GC) with nitrogen-phosphorous detector (NPD). The silica monolith gave better peak shape and intensity than the P-DVB monolith. Formulation of silica monolith with tetramethoxysilane (TMOS) as a sole initiator provided better separation and higher peak intensity, compared to those with methyltrimethoxysilane (MTMS) and (3:1) TMOS/MTMS initiators. The optimum internal diameter and length of silica monolith-capillary were 0.25 mm and 5 cm, respectively. The purge and trap conditions were optimised by purging with nitrogen and heating the honey sample solution at 100 °C for 60 min. Recovery of the method was in a range of 84.95-99.71% and the detection limits of the pesticides determined by using GC-NPD and GC-mass spectrometric detector (MSD) ranged between 0.36-1.75 and 0.13-0.25 ng g(-1), respectively.

  12. Kinetics and equilibria of the chromatographic separation of maltose and trehalose.

    PubMed

    He, Dengjun; Zhou, Jiachun; Xia, Quanming; Jiang, Lihua; Qiu, Yongjun; Zhao, Liming

    2015-07-01

    Trehalose, a nonreducing disaccharide, has been extensively applied to food, cosmetics, and pharmaceutical goods. The resultant solution of trehalose prepared by enzymatic methods includes high amounts of maltose. However, it is quite difficult to separate maltose and trehalose on an industrial scale because of their similar properties. In this paper, a high-performance resin was selected as a stationary phase to separate trehalose and maltose, and the resolution of these sugars was 0.59. The potential of a cation exchange resin was investigated as the stationary phase in separating trehalose and maltose using deionized water as the mobile phase. Based on the equilibrium dispersive model, the axial dispersion coefficients and overall mass transfer coefficients of maltose and trehalose were determined by moment analysis at two different temperatures, 50 and 70°C. Other parameters, including the column void and the adsorption isotherms, were also determined and applied to simulate the elution curves of trehalose and maltose. The simulated results matched the experimental data, validating the parameters. The optimized parameters are critical to the chromatographic separation of trehalose and maltose on an industrial scale.

  13. Adsorption of the antiepileptic carbamazepine onto agricultural soils.

    PubMed

    Calisto, Vania; Esteves, Valdemar I

    2012-05-01

    Carbamazepine is an antiepileptic pharmaceutical which is commonly found in environmental matrices. It passes through wastewater treatment plants (WWTPs) almost completely unaffected and has been found to be highly persistent in the environment. The application of sludge in agricultural fields and the use of WWTP effluents for irrigation constitute a potential source of soil contamination. Consequently, the assessment of the interaction between carbamazepine and soils is of crucial importance to understand its fate in the environment. To monitor the sorption behavior of carbamazepine onto agricultural soils, batch equilibrium experiments were performed using soils subjected to distinct long-term fertilizations. In order to follow the adsorption experiments, an UV spectral deconvolution methodology was applied and the results compared with those from micellar electrokinetic chromatography. The results obtained by both methods did not present significant statistical differences at 95% confidence level. Therefore, it was proven that, in the context of adsorption studies, UV spectral deconvolution is a valid alternative to common chromatographic methods, with the major advantage of being a simple and fast procedure. The adsorption of carbamazepine onto the selected soils was satisfactorily described by the Freundlich model. The obtained Freundlich parameters (K(F)) (between 1.79 ± 0.07 and 4.8 ± 0.2 mg kg(-1) (mg L(-1))(-N)) indicate that the adsorption behavior of carbamazepine is dependent on the soil fertilization. Also, it is not extensively sorbed, indicating that carbamazepine present in soils can be a potential source of contamination of surface and ground waters through run-off and infiltration.

  14. Unified superresolution experiments and stochastic theory provide mechanistic insight into protein ion-exchange adsorptive separations

    PubMed Central

    Kisley, Lydia; Chen, Jixin; Mansur, Andrea P.; Shuang, Bo; Kourentzi, Katerina; Poongavanam, Mohan-Vivekanandan; Chen, Wen-Hsiang; Dhamane, Sagar; Willson, Richard C.; Landes, Christy F.

    2014-01-01

    Chromatographic protein separations, immunoassays, and biosensing all typically involve the adsorption of proteins to surfaces decorated with charged, hydrophobic, or affinity ligands. Despite increasingly widespread use throughout the pharmaceutical industry, mechanistic detail about the interactions of proteins with individual chromatographic adsorbent sites is available only via inference from ensemble measurements such as binding isotherms, calorimetry, and chromatography. In this work, we present the direct superresolution mapping and kinetic characterization of functional sites on ion-exchange ligands based on agarose, a support matrix routinely used in protein chromatography. By quantifying the interactions of single proteins with individual charged ligands, we demonstrate that clusters of charges are necessary to create detectable adsorption sites and that even chemically identical ligands create adsorption sites of varying kinetic properties that depend on steric availability at the interface. Additionally, we relate experimental results to the stochastic theory of chromatography. Simulated elution profiles calculated from the molecular-scale data suggest that, if it were possible to engineer uniform optimal interactions into ion-exchange systems, separation efficiencies could be improved by as much as a factor of five by deliberately exploiting clustered interactions that currently dominate the ion-exchange process only accidentally. PMID:24459184

  15. Unified superresolution experiments and stochastic theory provide mechanistic insight into protein ion-exchange adsorptive separations.

    PubMed

    Kisley, Lydia; Chen, Jixin; Mansur, Andrea P; Shuang, Bo; Kourentzi, Katerina; Poongavanam, Mohan-Vivekanandan; Chen, Wen-Hsiang; Dhamane, Sagar; Willson, Richard C; Landes, Christy F

    2014-02-11

    Chromatographic protein separations, immunoassays, and biosensing all typically involve the adsorption of proteins to surfaces decorated with charged, hydrophobic, or affinity ligands. Despite increasingly widespread use throughout the pharmaceutical industry, mechanistic detail about the interactions of proteins with individual chromatographic adsorbent sites is available only via inference from ensemble measurements such as binding isotherms, calorimetry, and chromatography. In this work, we present the direct superresolution mapping and kinetic characterization of functional sites on ion-exchange ligands based on agarose, a support matrix routinely used in protein chromatography. By quantifying the interactions of single proteins with individual charged ligands, we demonstrate that clusters of charges are necessary to create detectable adsorption sites and that even chemically identical ligands create adsorption sites of varying kinetic properties that depend on steric availability at the interface. Additionally, we relate experimental results to the stochastic theory of chromatography. Simulated elution profiles calculated from the molecular-scale data suggest that, if it were possible to engineer uniform optimal interactions into ion-exchange systems, separation efficiencies could be improved by as much as a factor of five by deliberately exploiting clustered interactions that currently dominate the ion-exchange process only accidentally.

  16. Kafirin adsorption on ion-exchange resins: isotherm and kinetic studies.

    PubMed

    Kumar, Prashant; Lau, Pei Wen; Kale, Sandeep; Johnson, Stuart; Pareek, Vishnu; Utikar, Ranjeet; Lali, Arvind

    2014-08-22

    Kafirin is a natural, hydrophobic and celiac safe prolamin protein obtained from sorghum seeds. Today kafirin is found to be useful in designing delayed delivery systems and coatings of pharmaceuticals and nutraceuticals where its purity is important and this can be obtained by adsorptive chromatography. This study is the first scientific insight into the isotherm and kinetic studies of kafirin adsorption on anion- and cation-exchange resins for practical applications in preparative scale chromatography. Adsorption isotherms of kafirin were determined for five anion- and two cation-exchange resins in batch systems. Isotherm parameters such as maximum binding capacity and dissociation constant were determined from Langmuir isotherm, and adsorptive capacity and affinity constant from Freundlich isotherm. Langmuir isotherm was found to fit the adsorption equilibrium data well. Batch uptake kinetics for kafirin adsorption on these resins was also carried out and critical parameters including the diffusion coefficient, film mass transfer coefficient, and Biot number for film-pore diffusion model were calculated. Both the isotherm and the kinetic parameters were considered for selection of appropriate resin for kafirin purification. UNOsphere Q (78.26 mg/ml) and Toyopearl SP-650M (57.4 mg/ml) were found to offer better kafirin binding capacities and interaction strength with excellent uptake kinetics under moderate operating conditions. With these adsorbents, film diffusion resistance was found to be major governing factor for adsorption (Bi<10 and δ<1). Based on designer objective function, UNOsphere Q was found be best adsorbent for binding of kafirin. The data presented is valuable for designing large scale preparative adsorptive chromatographic kafirin purification systems.

  17. Trace adsorption of positively charged proteins onto Sepharose FF and Sepharose FF-based anion exchangers.

    PubMed

    Yu, Lin-Ling; Sun, Yan

    2012-08-31

    Agarose-based matrices have been widely used in ion exchange chromatography (IEC). We have herein observed that positively charged proteins (lysozyme and cytochrome c) are adsorbed on the agarose-based anion-exchangers (Q and DEAE Sepharose FF gels) in a capacity of 10-40 μg/mL. In contrast, negatively charged protein (bovine serum albumin) is not adsorbed to Sepharose FF and SP Sepharose FF gels. Elemental analysis of the gel indicated that the residual anionic sulfate groups in agarose would have worked as the cation exchange groups for the positively charged proteins. The trace adsorption behavior of lysozyme onto Sepharose FF and Sepharose FF-based anion exchangers was studied and the effects of NaCl concentration and cation group density on the adsorption were examined for better understanding of the trace adsorption in chromatographic processes. At NaCl concentrations less than 0.05 mol/L, which is the normal adsorption condition in IEC, the trace adsorption kept at a high level, so this trace adsorption cannot be avoided in the ionic strength range of routine IEC operations. Grafting poly(ethylenimine) (PEI) chain of 60 kDa to a cation group density of 700 mmol/L could reduce the adsorption capacity to about 20 μg/mL, but further reduction was not possible by increasing the cation group density to 1200 mmol/L. Therefore, attentions need to be paid to the phenomenon in protein purification practice using agarose-based matrices. The research is expected to call attentions to the trace adsorption on agarose-based matrices and to the importance in the selection of the suitable solid matrices in the production of high-purity protein products in large-scale bioprocesses.

  18. Adsorption of polyethylene-glycolated bovine serum albumin on macroporous and polymer-grafted anion exchangers.

    PubMed

    Zhu, Mimi; Carta, Giorgio

    2014-01-24

    The chromatographic and adsorptive properties of BSA and BSA conjugated with 10 and 30kDa PEG polymers are determined for a macroporous anion exchanger (UNOsphere™ Diol Q) and for a polymer-grafted material having the same backbone matrix (Nuvia Q™). Chromatographic retention, adsorption capacity, and adsorption kinetics are enhanced in the polymer-grafted resin for both BSA and 10kDa PEG-BSA as a result of interactions with the grafted polymers. However, the difference between the two resins diminishes for 30kDa PEG-BSA indicating that size exclusion effects strongly affect binding in the polymer-grafted material for this larger conjugate. Images of intraparticle concentration profiles obtained by confocal scanning laser microscopy show that the transport mechanisms of both BSA and PEGylated BSA are very different in the two resins. The protein binding kinetics are dominated by ordinary pore diffusion and are essentially independent of the direction of transport for UNOsphere Diol Q as a result of its large pore size. Thus, for this material, displacement of PEGylated BSA by BSA is clearly evident at the intraparticle scale. On the other hand, the protein binding kinetics in Nuvia Q are consistent with a solid diffusion mechanism driven by the adsorbed protein concentration. For this material, protein transport is very fast for one component or two-component co-adsorption of BSA and PEGylated BSA but slows down dramatically for sequential adsorption of these species as a result of heightened diffusional hindrance when the two components counterdiffuse within the resin.

  19. Theoretical study of the accuracy of the pulse method, frontal analysis, and frontal analysis by characteristic points for the determination of single component adsorption isotherms

    SciTech Connect

    Kaczmarski, Krzysztof; Guiochon, Georges A

    2009-01-01

    The adsorption isotherms of selected compounds are our main source of information on the mechanisms of adsorption processes. Thus, the selection of the methods used to determine adsorption isotherm data and to evaluate the errors made is critical. Three chromatographic methods were evaluated, frontal analysis (FA), frontal analysis by characteristic point (FACP), and the pulse or perturbation method (PM), and their accuracies were compared. Using the equilibrium-dispersive (ED) model of chromatography, breakthrough curves of single components were generated corresponding to three different adsorption isotherm models: the Langmuir, the bi-Langmuir, and the Moreau isotherms. For each breakthrough curve, the best conventional procedures of each method (FA, FACP, PM) were used to calculate the corresponding data point, using typical values of the parameters of each isotherm model, for four different values of the column efficiency (N = 500, 1000, 2000, and 10,000). Then, the data points were fitted to each isotherm model and the corresponding isotherm parameters were compared to those of the initial isotherm model. When isotherm data are derived with a chromatographic method, they may suffer from two types of errors: (1) the errors made in deriving the experimental data points from the chromatographic records; (2) the errors made in selecting an incorrect isotherm model and fitting to it the experimental data. Both errors decrease significantly with increasing column efficiency with FA and FACP, but not with PM.

  20. Accuracy of peak deconvolution algorithms within chromatographic integrators

    SciTech Connect

    Papas, A.N. ); Tougas, T.P. )

    1990-02-01

    The soundness of present-day algorithms to deconvolve overlapping skewed peaks was investigated. From simulated studies based on the exponentially modified Gaussian model (EMG), chromatographic peak area inaccuracies for unresolved peaks are presented for the two deconvolution methods, the tangent skim and the perpendicular drop method. These inherent inaccuracies, in many cases exceeding 50%, are much greater than those calculated from ideal Gaussian profiles. Multiple linear regression (MLR) was used to build models that predict the relative error for either peak deconvolution method. MLR also provided a means for determining influential independent variables, defining the required chromatographic relationships needed for prediction. Once forecasted errors for both methods are calculated, selection of either peak deconvolution method can be made by minimum errors. These selection boundaries are contrasted to method selection criteria of present data systems algorithms.

  1. Catalytically-Promoted Analyte Derivatization Inside a Gas Chromatographic Inlet

    PubMed Central

    Fowler, William K.; Gamble, Kelly J.; Wright, Amber R.

    2010-01-01

    Reported here is a preliminary assessment of the feasibility of catalyzing on-line derivatization reactions inside the inlet (i.e., the injection port) of a gas chromatograph (GC) with solid heterogeneous catalysts. The experiments described here entail the installation of candidate catalysts inside the GC inlet liner and the subsequent injection of analyte/reagent mixtures onto the catalyst beds. Two catalysts are identified, each of which clearly catalyzes one of the chosen model derivatization reactions in the inlet of a GC. This result supports our hypothesis that on-line derivatizations can, in principle, be reproducibly catalyzed inside the GC inlet by solid heterogeneous catalysts and that the presence of such catalysts in the inlet do not necessarily cause a serious loss of instrument performance or chromatographic efficiency. PMID:20822662

  2. Intercalibration of chromatographic methods for auxino phytodrugs in Solanaceae.

    PubMed

    Gennaro, M C; Marengo, E; Gianotti, V; Angioi, S; Copeta, G

    2003-04-18

    Three chromatographic methods are considered for the determination in Solanaceae of auxino-similar phytodrugs, so called because their structure resembles an auxine plant hormone. The phytodrugs studied were: 2,4-dichlorophenoxyacetic acid, 2,4-dichlorophenoxypropionic acid, 2,4-dichlorophenoxybutyric acid, 2-methyl-4-chlorophenoxyacetic acid, 2,4,5-trichlorophenoxyacetic acid, naphthylacetic acid and 2-naphthyloxyacetic acid. Three chromatographic methods, respectively based on ion-interaction HPLC, GC-MS with intra-injector derivatisation and CC-MS with pre-injection derivatisation, were developed, optimised and validated. A comparative discussion of the advantages/disadvantages of the methods suggests a strategy for their preferential use, that is essentially a function of the matrix complexity.

  3. Techniques of preparing plant material for chromatographic separation and analysis.

    PubMed

    Romanik, G; Gilgenast, E; Przyjazny, A; Kamiński, M

    2007-03-10

    This paper discusses preparation techniques of samples of plant material for chromatographic analysis. Individual steps of the procedures used in sample preparation, including sample collection from the environment or from tissue cultures, drying, comminution, homogenization, leaching, extraction, distillation and condensation, analyte enrichment, and obtaining the final extracts for chromatographic analysis are discussed. The techniques most often used for isolation of analytes from homogenized plant material, i.e., Soxhlet extraction, ultrasonic solvent extraction (sonication), accelerated solvent extraction, microwave-assisted extraction, supercritical-fluid extraction, steam distillation, as well as membrane processes are emphasized. Sorptive methods of sample enrichment and removal of interferences, i.e., solid-phase extraction, and solid-phase micro-extraction are also discussed.

  4. Micro-column plasma emission liquid chromatograph. [Patent application

    DOEpatents

    Gay, D.D.

    1982-08-12

    In a direct current plasma emission spectrometer for use in combination with a microcolumn liquid chromatograph, an improved plasma source unit is claimed. The plasma source unit includes a quartz capillary tube having an inlet means, outlet off gas means and a pair of spaced electrodes defining a plasma region in the tube. The inlet means is connected to and adapted to receive eluant of the liquid chromatograph along with a stream of plasma-forming gas. There is an opening through the wall of the capillary tube penetrating into the plasma region. A soft glass capillary light pipe is disposed at the opening, is connected to the spectrometer, and is adapted to transmit light passing from the plasma region to the spectrometer. There is also a source of electromotive force connected to the electrodes sufficient to initiate and sustain a plasma in the plasma region of the tube.

  5. The chromatographic behaviour of wasp venom kinin, kallidin and bradykinin.

    PubMed

    MATHIAS, A P; SCHACHTER, M

    1958-09-01

    Wasp venom kinin which has hitherto appeared to be homogeneous can be resolved by ionexchange chromatography into a single major and two minor components. These are indistinguishable by their action on smooth muscle and by their rapid inactivation by chymotrypsin. All three components of wasp kinin are chromatographically different from kallidin or bradykinin. The close similarity of the latter compounds is confirmed by their identical behaviour on an ion-exchange resin.

  6. Can enantiomers be separated in achiral chromatographic systems?

    NASA Astrophysics Data System (ADS)

    Davankov, V. A.

    2016-10-01

    Consideration of chromatography of a nonracemic mixture on an achiral sorbent from a stereochemical point of view allows the claim that partial separation of the excess enantiomer zone from the racemate zone is possible only with analytes capable of self-associating under the conditions of the chromatographic column. It is from these positions that features of this process can be explained and conditions for its maximal proceeding formulated.

  7. Metal-Organic Frameworks for Thin-Layer Chromatographic Applications.

    PubMed

    Schenk, Claudia; Kutzscher, Christel; Drache, Franziska; Helten, Stella; Senkovska, Irena; Kaskel, Stefan

    2017-01-25

    Preparation of thin-layer chromatographic (TLC) plates based on metal-organic frameworks (MOFs) as porous stationary phases is described. DUT-67 (DUT = Dresden University of Technology), a zirconium based MOF, was used in combination with a fluorescent indicator as stationary phase for analyzing a small selection of a wide spectrum of relevant analytes. The successful separation of benzaldehyde from trans-cinnamaldehyde and 4-aminophenol from 2-aminotoluene is reported as a model system using optimized eluent mixtures containing acetic acid.

  8. Prediction of pesticides chromatographic lipophilicity from the computational molecular descriptors.

    PubMed

    Casoni, Dorina; Petre, Jana; David, Victor; Sârbu, Costel

    2011-02-01

    Quantitative structure-property relationship models were developed for the prediction of pesticides and some PAH compounds lipophilicity based on a wide set of computational molecular descriptors and a set of experimental chromatographic data. The chromatographic lipophilicity of pesticides has been evaluated by high-performance liquid chromatography (HPLC) using different chemically bonded (C18, C8, CN and Phenyl HPLC columns) stationary phases and two different organic modifiers (methanol and acetonitrile, respectively) in the mobile phase composition. Through a systematic study, by using the classic multivariate analysis, several quantitative structure-property/lipophilicity multi-dimensional models were established. Multiple linear regression and genetic algorithm for the variable subset selection were used. The internal and external statistical evaluation procedures revealed some appropriate models for the chromatographic lipophilicity prediction of pesticides. Moreover, the statistical parameters of regression and those obtained by applying t-test for the intercept (a(0)) and for the slope (a(1)) in order to evaluate relationship between experimental and predicted octanol-water partition coefficients in case of the test set compounds, revealed two statistically valid models that can be successfully used in lipophilicity prediction of pesticides.

  9. Development of a simple technique for the coating of monolithic silica with pristine boron nitride nanotubes (BNNTs): HPLC chromatographic applications.

    PubMed

    Guillaume, Yves Claude; André, Claire

    2017-03-01

    In this paper, a novel and very simple homogeneous coating of a monolithic silica HPLC support using pristine boron nitride nanotubes (BNNTs) was d0.escribed. The chromatographic support was coated with BNNTs in a non covalent way to preserve the nanotube structure. A solution of BNNTs dispersed in dimethylacetamide (DMAc) was pumped through the column at a flow-rate of 0.3mL/min for 24h at room temperature. Strong interaction between amino groups and the BNNT surfaces induces the adsorption of the BNNTs on the silica, while the stable solvation in DMAc hampers further adsorption of the tubes. The excellent stability of the non covalent BNNT-coating on the monolithic silica in view of application for HPLC was also demonstrated. It was shown that this novel stationary phase was efficient for the HPLC isocratic or gradient mode separation of molecules of different structure such as phenol derivatives, alkylbenzene or doping agents (steroids). As well, this simple technique of BNNT immobilization offers new perspectives for the BNNT-coating on the surfaces of a wide range of solid substrates.

  10. Single-walled carbon nanotubes as stationary phase in gas chromatographic separation and determination of argon, carbon dioxide and hydrogen.

    PubMed

    Safavi, Afsaneh; Maleki, Norooz; Doroodmand, Mohammad Mahdi

    2010-08-24

    A chromatographic technique is introduced based on single-walled carbon nanotubes (SWCNTs) as stationary phase for separation of Ar, CO(2) and H(2) at parts per million (ppm) levels. The efficiency of SWCNTs was compared with solid materials such as molecular sieve, charcoal, multi-walled carbon nanotubes and carbon nanofibers. The morphology of SWCNTs was optimized for maximum adsorption of H(2), CO(2) and Ar and minimum adsorption of gases such as N(2), O(2), CO and H(2)O vapour. To control temperature of the gas chromatography column, peltier cooler was used. Mixtures of Ar, CO(2) and H(2) were separated according to column temperature program. Relative standard deviation for nine replicate analyses of 0.2 mL H(2) containing 10 microL of each Ar or CO(2) was 2.5% for Ar, 2.8% for CO(2) and 3.6% for H(2). The interfering effects of CO, and O(2) were investigated. Working ranges were evaluated as 40-600 ppm for Ar, 30-850 ppm for CO(2) and 10-1200 ppm for H(2). Significant sensitivity, small relative standard deviation (RSD) and acceptable limit of detection (LOD) were obtained for each analyte, showing capability of SWCNTs for gas separation and determination processes. Finally, the method was used to evaluate the contents of CO(2) in air sample.

  11. Liquid-Phase Adsorption Fundamentals.

    ERIC Educational Resources Information Center

    Cooney, David O.

    1987-01-01

    Describes an experiment developed and used in the unit operations laboratory course at the University of Wyoming. Involves the liquid-phase adsorption of an organic compound from aqueous solution on activated carbon, and is relevant to adsorption processes in general. (TW)

  12. Chromium adsorption by lignin

    SciTech Connect

    Lalvani, S.B.; Huebner, A.; Wiltowski, T.S.

    2000-01-01

    Hexavalent chromium is a known carcinogen, and its maximum contamination level in drinking water is determined by the US Environmental Protection Agency (EPA). Chromium in the wastewaters from plating and metal finishing, tanning, and photographic industries poses environmental problems. A commercially available lignin was used for the removal of hexavalent as well as trivalent chromium from aqueous solution. It is known that hexavalent chromium is present as an anionic species in the solution. It was found that lignin can remove up to 63% hexavalent and 100% trivalent chromium from aqueous solutions. The removal of chromium ions was also investigated using a commercially available activated carbon. This absorbent facilitated very little hexavalent and almost complete trivalent chromium removal. Adsorption isotherms and kinetics data on the metal removal by lignin and activated carbon are presented and discussed.

  13. High temperature adsorption measurements

    SciTech Connect

    Bertani, R.; Parisi, L.; Perini, R.; Tarquini, B.

    1996-12-31

    Adsorption phenomena are a rich and rather new field of study in geothermal research, in particular at very high temperature. ENEL is interested in the exploitation of geothermal regions with super-heated steam, and it is important to understand the behavior of water-rock interaction. We have analyzed in the 170-200{degrees}C temperature range four samples of Monteverdi cuttings; the next experimental effort will be at 220{degrees}C and over in 1996. The first results of the 1995 runs are collected in this paper. We can highlight four main items: (1) At relative pressures over 0.6 the capillarity forces are very important. (2) There is no significant temperature effect. (3) Adsorbed water can be present, and it is able to multiply by a factor of 15 the estimated reserve of super-heated steam only. (4) Pores smaller than 15 {Angstrom} do not contribute to the adsorbed mass.

  14. High temperature adsorption measurements

    SciTech Connect

    Bertani, R.; Parisi, L.; Perini, R.; Tarquini, B.

    1996-01-24

    Adsorption phenomena are a rich and rather new field of study in geothermal research, in particular at very high temperature. ENEL is interested in the exploitation of geothermal regions with superheated steam, and it is important to understand the behavior of water-rock interaction. We have analyzed in the 170-200 °C temperature range four samples of Monteverdi cuttings; the next experimental effort will be at 220 °C and over in 1996. The first results of the 1995 runs are collected in this paper. We can highlight four main items: 1. At relative pressures over 0.6 the capillarity forces are very important. 2. There is no significant temperature effect. 3. Adsorbed water can be present, and it is able to multiply by a factor of 15 the estimated reserve of super-heated steam only. 4. Pores smaller than 15 Å do not contribute to the adsorbed mass.

  15. Protein adsorption to poly(ethylenimine)-modified Sepharose FF. IV. Dynamic adsorption and elution behaviors.

    PubMed

    Liu, Na; Yu, Lin-Ling; Sun, Yan

    2014-10-03

    We have previously investigated bovine serum albumin (BSA) uptake to poly(ethylenimine) (PEI)-grafted Sepharose FF. It was found that there was a critical ionic capacity (cIC; 600mmol/L) for BSA, above which the protein adsorption capacity and uptake kinetics increased drastically. In this work, two poly(ethylenimine) (PEI)-grafted resins with IC values of 271mmol/L (FF-PEI-L270) and 683mmol/L (FF-PEI-L680), which were below and above the cIC, respectively, were chosen to investigate the breakthrough and linear gradient elution (LGE) behaviors of BSA. Commercially available anion exchanger, Q Sepharose FF, was used for comparison. The DBC values of FF-PEI-L680 were much higher in the entire residence time range (2-10min) than the other two resins due to its high static adsorption capacity and uptake kinetics. At a residence time of 5.0min, the DBC of FF-PEI-L680 (104mg/mL) was about seven times that of FF-PEI-L270 and three times that of Q Sepharose FF. A rise-fall trend of the DBCs with increasing ionic strength (IS) was found for all the three resins studied, indicating the presence of electrostatic exclusion for protein uptake at low IS. With increasing NaCl concentration from 20 to 200mmol/L, FF-PEI-L680 kept very high DBC values (64-114mg/mL). In addition, FF-PEI-L270 showed more favorable adsorption properties than Q Sepharose FF at 100-300mmol/L NaCl. These results proved that the three-dimensional grafting ion exchange layer on the PEI resins enhanced their tolerance to IS. In the study of LGE, the three resins showed similar elution behaviors and no distinct peak tailings were observed. The salt concentrations at the elution peaks (IR) were in the order of FF-PEI-L680>FF-PEI-L270>Q Sepharose FF, indicating that the elution for the PEI resins needed higher salt concentrations, which was also an appearance of the salt-tolerant feature of the PEI resins. When protein loading amount was increased to the value equivalent to the DBC at 10% breakthrough, the

  16. Random sequential adsorption on fractals.

    PubMed

    Ciesla, Michal; Barbasz, Jakub

    2012-07-28

    Irreversible adsorption of spheres on flat collectors having dimension d < 2 is studied. Molecules are adsorbed on Sierpinski's triangle and carpet-like fractals (1 < d < 2), and on general Cantor set (d < 1). Adsorption process is modeled numerically using random sequential adsorption (RSA) algorithm. The paper concentrates on measurement of fundamental properties of coverages, i.e., maximal random coverage ratio and density autocorrelation function, as well as RSA kinetics. Obtained results allow to improve phenomenological relation between maximal random coverage ratio and collector dimension. Moreover, simulations show that, in general, most of known dimensional properties of adsorbed monolayers are valid for non-integer dimensions.

  17. Galactose adsorption on Ru(0001)

    NASA Astrophysics Data System (ADS)

    Alatalo, Matti; Puisto, Mikko

    2014-03-01

    In order to understand the valorisation of biomass, it is essential to study the behavior of sugar molecules on catalytic surfaces. We have studied the adsorption of galactose molecules on the Ru(0001) surface using first principles calculations. We present results for the fully relaxed configurations of the molecule at different adsorption sites. We also compare the effect of the inclusion of the van der Waals interactions on both the energetics of the free galactose molecule and the adsorption energy of galactose on Ru(0001). We compare our results, obtained using periodically repeated supercells, to those obtained with cluster calculations.

  18. Protein Adsorption in Three Dimensions

    PubMed Central

    Vogler, Erwin A.

    2011-01-01

    Recent experimental and theoretical work clarifying the physical chemistry of blood-protein adsorption from aqueous-buffer solution to various kinds of surfaces is reviewed and interpreted within the context of biomaterial applications, especially toward development of cardiovascular biomaterials. The importance of this subject in biomaterials surface science is emphasized by reducing the “protein-adsorption problem” to three core questions that require quantitative answer. An overview of the protein-adsorption literature identifies some of the sources of inconsistency among many investigators participating in more than five decades of focused research. A tutorial on the fundamental biophysical chemistry of protein adsorption sets the stage for a detailed discussion of the kinetics and thermodynamics of protein adsorption, including adsorption competition between two proteins for the same adsorbent immersed in a binary-protein mixture. Both kinetics and steady-state adsorption can be rationalized using a single interpretive paradigm asserting that protein molecules partition from solution into a three-dimensional (3D) interphase separating bulk solution from the physical-adsorbent surface. Adsorbed protein collects in one-or-more adsorbed layers, depending on protein size, solution concentration, and adsorbent surface energy (water wettability). The adsorption process begins with the hydration of an adsorbent surface brought into contact with an aqueous-protein solution. Surface hydration reactions instantaneously form a thin, pseudo-2D interface between the adsorbent and protein solution. Protein molecules rapidly diffuse into this newly-formed interface, creating a truly 3D interphase that inflates with arriving proteins and fills to capacity within milliseconds at mg/mL bulk-solution concentrations CB. This inflated interphase subsequently undergoes time-dependent (minutes-to-hours) decrease in volume VI by expulsion of either-or-both interphase water and

  19. Rotating annular chromatograph for continuous metal separations and recovery

    SciTech Connect

    Begovich, J.M.; Sisson, W.G.

    1981-01-01

    Multicomponent liquid chromatographic separations have been achieved by using a slowly rotating annular bed of sorbent material. By continuously introducing the feed material to be separated at a stationary point at the top of the bed and eluent everywhere else around the annulus, elution chromatography occurs. The rotation of the sorbent bed causes the separated components to appear as helical bands, each of which has a characteristic, stationary exit point; hence, the separation process is truly continuous. The concept has been developed primarily on a 279-mm-diam by 0.6-m-long device with a 12.7-mm-wide annulus. The effect of annulus width and diameter has recently been studied using the same device with a 50.8-mm-wide annulus and another 0.6-m-long chromatograph with an 89-mm diameter and annulus widths of 6.4, 12.7, and 22.2 mm. These columns have been constructed of Plexiglas and typically operate at a gauge pressure of 175 kPa. To further study the effect of size and pressure, a new 445-mm-diam by 1-m-long column with a 31.8-mm-wide annulus has been fabricated. Its metal construction allows preparative-scale operation with a wide variety of liquids at pressures to 1.3 MPa. Three metal recovery systems have been explored: (1) separation of iron and aluminum in ammonium sulfate-sulfuric acid solutions; (2) separation of hafnium from zirconium in sulfuric acid solutions; and (3) the separation of copper, nickel, and cobalt in ammonium carbonate solutions. This last system simulates the leach liquor of the Caron process for recovering nickel and cobalt from laterite ores. It has been studied, using similar conditions, on each of the chromatographs, and the results demonstrate the effect of column dimensions on the quality and quantity of the separation. 8 figures, 1 table.

  20. Liquid chromatographic determination of pyrantel tartrate in medicated formulations.

    PubMed

    Konrardy, Joyce A; Burner, Mary A; Garner, Tommy W; Litchman, Mark A; Webster, Gregory K

    2003-01-01

    The validation of a novel liquid chromatographic (LC) method for the determination of pyrantel tartrate in feed is presented. The method provides a significant improvement over the efficiency and precision of AOAC Official Method 978.30. The method was shown to be accurate, precise, linear, and robust for medicated articles. Unlike the official method, the LC method was shown to be a superior stability-indicating method. After the method was validated by using laboratory blends, the effectiveness of the method was demonstrated with marketed product as well.

  1. Gas chromatographic analysis of trace gas impurities in tungsten hexafluoride.

    PubMed

    Laurens, J B; de Coning, J P; Swinley, J M

    2001-03-09

    Highly reactive fluorinated gaseous matrices require special equipment and techniques for the gas chromatographic analysis of trace impurities in these gases. The impurities that were analysed at the low-microg/l levels included oxygen, nitrogen, carbon dioxide, carbon monoxide, sulfur hexafluoride and hydrogen. This paper describes the use of a system utilising backflush column switching to protect the columns and detectors in the analysis of trace gas impurities in tungsten hexafluoride. Two separate channels were used for the analysis of H2, O2, N2, CO, CO2 and SF6 impurities with pulsed discharge helium ionisation detection.

  2. Methods and apparatus for analysis of chromatographic migration patterns

    DOEpatents

    Stockham, Thomas G.; Ives, Jeffrey T.

    1993-01-01

    A method and apparatus for sharpening signal peaks in a signal representing the distribution of biological or chemical components of a mixture separated by a chromatographic technique such as, but not limited to, electrophoresis. A key step in the method is the use of a blind deconvolution technique, presently embodied as homomorphic filtering, to reduce the contribution of a blurring function to the signal encoding the peaks of the distribution. The invention further includes steps and apparatus directed to determination of a nucleotide sequence from a set of four such signals representing DNA sequence data derived by electrophoretic means.

  3. Methods and apparatus for analysis of chromatographic migration patterns

    DOEpatents

    Stockham, T.G.; Ives, J.T.

    1993-12-28

    A method and apparatus are presented for sharpening signal peaks in a signal representing the distribution of biological or chemical components of a mixture separated by a chromatographic technique such as, but not limited to, electrophoresis. A key step in the method is the use of a blind deconvolution technique, presently embodied as homomorphic filtering, to reduce the contribution of a blurring function to the signal encoding the peaks of the distribution. The invention further includes steps and apparatus directed to determination of a nucleotide sequence from a set of four such signals representing DNA sequence data derived by electrophoretic means. 16 figures.

  4. Cation exchange chromatographic elution and separation of rubidium

    SciTech Connect

    Mehta, V.P.; Khopkar, S.M.

    1982-01-01

    The systematic cation exchange chromatographic separation of rubidium on Dowex 50W-X8 was carried out with mineral acids and their salts as eluants.A selectivity scale for various eluants in terms of the elution constant was devised. Rubidium was separated from a large number of elements in binary mixtures by the process of gradient or selective elutions or selective sorption. The noteworthy feature of the method is the sequential separation of rubidium from alkali as well as alkaline earth elements.

  5. Bromide Adsorption by Reference Minerals and Soils

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Bromide, Br-, adsorption behavior was investigated on amorphous Al and Fe oxide, montmorillonite, kaolinite, and temperate and tropical soils. Bromide adsorption decreased with increasing solution pH with minimal adsorption occurring above pH 7. Bromide adsorption was higher for amorphous oxides t...

  6. Centrifugal Adsorption Cartridge System

    NASA Technical Reports Server (NTRS)

    Gonda, Steve R.; Tsao, Yow-Min D.; Lee, Wenshan

    2004-01-01

    The centrifugal adsorption cartridge system (CACS) is an apparatus that recovers one or more bioproduct(s) from a dilute aqueous solution or suspension flowing from a bioreactor. The CACS can be used both on Earth in unit gravity and in space in low gravity. The CACS can be connected downstream from the bioreactor; alternatively, it can be connected into a flow loop that includes the bioreactor so that the liquid can be recycled. A centrifugal adsorption cartridge in the CACS (see figure) includes two concentric cylinders with a spiral ramp between them. The volume between the inner and outer cylinders, and between the turns of the spiral ramp is packed with an adsorbent material. The inner cylinder is a sieve tube covered with a gas-permeable, hydrophobic membrane. During operation, the liquid effluent from the bioreactor is introduced at one end of the spiral ramp, which then constrains the liquid to flow along the spiral path through the adsorbent material. The spiral ramp also makes the flow more nearly uniform than it would otherwise be, and it minimizes any channeling other than that of the spiral flow itself. The adsorbent material is formulated to selectively capture the bioproduct(s) of interest. The bioproduct(s) can then be stored in bound form in the cartridge or else eluted from the cartridge. The centrifugal effect of the spiral flow is utilized to remove gas bubbles from the liquid. The centrifugal effect forces the bubbles radially inward, toward and through the membrane of the inner cylinder. The gas-permeable, hydrophobic membrane allows the bubbles to enter the inner cylinder while keeping the liquid out. The bubbles that thus enter the cylinder are vented to the atmosphere. The spacing between the ramps determines rate of flow along the spiral, and thereby affects the air-bubble-removal efficiency. The spacing between the ramps also determines the length of the fluid path through the cartridge adsorbent, and thus affects the bioproduct

  7. Evaluation of Gas Chromatographic Methods for Analysis of Gasoline/Oxygenate Blends.

    DTIC Science & Technology

    1981-12-01

    determination of various oxygenated compounds in gasoline by gas chromotography have been developed.(3-6) These include gas chromatographic (GC) analysis of the...ID-Ai33 0i6 EVALUATION OF GAS CHROMATOGRAPHIC METHODS FOR ANALYSIS i/t OF GASOLINE/OXYGEN.. (U) SOUTHWEST RESEARCH INST SAN ANTONIO TX ARMY FUELS...0 EVALUATION OF GAS -CHROMATOGRAPHIC METHODS FOR ANALYSIS OF GASOLINE/OXYGENATE BLENDS INTERIM REPORT

  8. Application of XAD-2 resin-based passive samplers and SPME-GC-MS/MS analysis for the monitoring of spatial and temporal variations of atmospheric pesticides in Luxembourg.

    PubMed

    Schummer, Claude; Tuduri, Ludovic; Briand, Olivier; Appenzeller, Brice M; Millet, Maurice

    2012-11-01

    Passive air sampling has been shown to be a very interesting alternative to high-volume sampling by overcoming its disadvantages (size, weight, expensiveness). However, to date, only limited data is available about passive air sampling of current-use pesticides. In order to test if passive samplers allow monitoring of spatial and temporal variations of atmospheric pesticide concentrations, five XAD-2-resin based passive air samplers were deployed at five locations in Luxembourg. Samplers were analyzed using accelerated solvent extraction coupled to solid-phase microextraction and gas chromatography with tandem mass spectrometry. Collected data was used to study the spatial and temporal variations of the concentrations of the compounds. Twenty two pesticides were detected between March and October, while no pesticides were detected from November to February. Highest concentrations were measured on the rural sites, suggesting that the used XAD-2 resin-based passive samplers allow the simultaneous monitoring of multiple current-use pesticides and identifying spatial and temporal variations.

  9. Short-Cycle Adsorption Refrigerator

    NASA Technical Reports Server (NTRS)

    Chan, C. K.

    1988-01-01

    Modular adsorption/Joule-Thomson-effect refrigerator offers fast regeneration; adsorption/desorption cycle time expected to be 1 minute. Pressurized hydrogen generated by bank of compressor modules during heating phase passes through system of check valves and expands in Joule-Thomson junction as it enters refrigeration chamber. Hydrogen absorbs heat from load before it is sucked out by another bank of compressor modules in cooling phase.

  10. Adsorption hysteresis in nanopores

    PubMed

    Neimark; Ravikovitch; Vishnyakov

    2000-08-01

    Capillary condensation hysteresis in nanopores is studied by Monte Carlo simulations and the nonlocal density functional theory. Comparing the theoretical results with the experimental data on low temperature sorption of nitrogen and argon in cylindrical channels of mesoporous siliceous molecular sieves of MCM-41 type, we have revealed four qualitatively different sorption regimes depending on the temperature and pore size. As the pore size increases at a given temperature, or as the temperature decreases at a given pore size, the following regimes are consequently observed: volume filling without phase separation, reversible stepwise capillary condensation, irreversible capillary condensation with developing hysteresis, and capillary condensation with developed hysteresis. We show that, in the regime of developed hysteresis (pores wider than 5 nm in the case of nitrogen sorption at 77 K), condensation occurs spontaneously at the vaporlike spinodal while desorption takes place at the equilibrium. A quantitative agreement is found between the modeling results and the experimental hysteresis loops formed by the adsorption-desorption isotherms. The results obtained provide a better understanding of the general behavior of confined fluids and the specifics of sorption and phase transitions in nanomaterials.

  11. Improving stability of virus-like particles by ion-exchange chromatographic supports with large pore size: advantages of gigaporous media beyond enhanced binding capacity.

    PubMed

    Yu, Mengran; Li, Yan; Zhang, Songping; Li, Xiunan; Yang, Yanli; Chen, Yi; Ma, Guanghui; Su, Zhiguo

    2014-02-28

    Limited binding capacity and low recovery of large size multi-subunits virus-like particles (VLPs) in conventional agarose-gel based chromatographic supports with small pores have long been a bottleneck limiting the large scale purification and application of VLPs. In this study, four anion exchange media including DEAE-Sepharose FF (DEAE-FF), DEAE-Capto, gigaporous DEAE-AP-120nm and DEAE-AP-280nm with average pore diameters of 32nm, 20nm, 120nm and 280nm, respectively, were applied for purification of hepatitis B virus surface antigen (HBsAg) VLPs. Pore size effects of media on the VLPs adsorption equilibrium, adsorption kinetics, dynamic binding capacity (DBC), and recovery were investigated in detail. According to the confocal laser scanning microscopy observation, adsorption of the VLPs in DEAE-FF and DEAE-Capto was mostly confined to a thin shell on the outer surface of the beads, leaving the underlying pore space and the binding sites inaccessibly, while the large pores in gigaporous media enabled the VLPs to access to the interior pore spaces by diffusion transport efficiently. Compared to the most widely used DEAE-FF, gigaporous media DEAE-AP-280nm gained about 12.9 times increase in static adsorption capacity, 8.0 times increase in DBC, and 11.4 times increase in effective pore diffusivity. Beyond increasing the binding capacity and enhancing the mass transfer, the gigaporous structure also significantly improved the stability of the VLPs during intensive adsorption-desorption process by lowing the multi-point interaction between the VLPs and binding sites in the pores. At 2.0mg/mL-media loading quantity, about 85.5% VLPs were correctly self-assembled after the chromatography with DEAE-AP-280nm media; oppositely about 85.2% VLPs lost their normal assembly with DEAE-FF due to irreversible disassembly. Comparative investigation was made to study the purifying performance of these four chromatographic media for actual VLPs purification from recombinant

  12. Surfactant adsorption kinetics in microfluidics

    PubMed Central

    Riechers, Birte; Maes, Florine; Akoury, Elias; Semin, Benoît; Gruner, Philipp; Baret, Jean-Christophe

    2016-01-01

    Emulsions are metastable dispersions. Their lifetimes are directly related to the dynamics of surfactants. We design a microfluidic method to measure the kinetics of adsorption of surfactants to the droplet interface, a key process involved in foaming, emulsification, and droplet coarsening. The method is based on the pH decay in the droplet as a direct measurement of the adsorption of a carboxylic acid surfactant to the interface. From the kinetic measurement of the bulk equilibration of the pH, we fully determine the adsorption process of the surfactant. The small droplet size and the convection during the droplet flow ensure that the transport of surfactant through the bulk is not limiting the kinetics of adsorption. To validate our measurements, we show that the adsorption process determines the timescale required to stabilize droplets against coalescence, and we show that the interface should be covered at more than 90% to prevent coalescence. We therefore quantitatively link the process of adsorption/desorption, the stabilization of emulsions, and the kinetics of solute partitioning—here through ion exchange—unraveling the timescales governing these processes. Our method can be further generalized to other surfactants, including nonionic surfactants, by making use of fluorophore–surfactant interactions. PMID:27688765

  13. Surfactant adsorption kinetics in microfluidics

    NASA Astrophysics Data System (ADS)

    Riechers, Birte; Maes, Florine; Akoury, Elias; Semin, Benoît; Gruner, Philipp; Baret, Jean-Christophe

    2016-10-01

    Emulsions are metastable dispersions. Their lifetimes are directly related to the dynamics of surfactants. We design a microfluidic method to measure the kinetics of adsorption of surfactants to the droplet interface, a key process involved in foaming, emulsification, and droplet coarsening. The method is based on the pH decay in the droplet as a direct measurement of the adsorption of a carboxylic acid surfactant to the interface. From the kinetic measurement of the bulk equilibration of the pH, we fully determine the adsorption process of the surfactant. The small droplet size and the convection during the droplet flow ensure that the transport of surfactant through the bulk is not limiting the kinetics of adsorption. To validate our measurements, we show that the adsorption process determines the timescale required to stabilize droplets against coalescence, and we show that the interface should be covered at more than 90% to prevent coalescence. We therefore quantitatively link the process of adsorption/desorption, the stabilization of emulsions, and the kinetics of solute partitioning—here through ion exchange—unraveling the timescales governing these processes. Our method can be further generalized to other surfactants, including nonionic surfactants, by making use of fluorophore-surfactant interactions.

  14. Multi-objective optimization of chromatographic rare earth element separation.

    PubMed

    Knutson, Hans-Kristian; Holmqvist, Anders; Nilsson, Bernt

    2015-10-16

    The importance of rare earth elements in modern technological industry grows, and as a result the interest for developing separation processes increases. This work is a part of developing chromatography as a rare earth element processing method. Process optimization is an important step in process development, and there are several competing objectives that need to be considered in a chromatographic separation process. Most studies are limited to evaluating the two competing objectives productivity and yield, and studies of scenarios with tri-objective optimizations are scarce. Tri-objective optimizations are much needed when evaluating the chromatographic separation of rare earth elements due to the importance of product pool concentration along with productivity and yield as process objectives. In this work, a multi-objective optimization strategy considering productivity, yield and pool concentration is proposed. This was carried out in the frame of a model based optimization study on a batch chromatography separation of the rare earth elements samarium, europium and gadolinium. The findings from the multi-objective optimization were used to provide with a general strategy for achieving desirable operation points, resulting in a productivity ranging between 0.61 and 0.75 kgEu/mcolumn(3), h(-1) and a pool concentration between 0.52 and 0.79 kgEu/m(3), while maintaining a purity above 99% and never falling below an 80% yield for the main target component europium.

  15. Gas chromatographic retention characteristics of phenols with Superox-20M

    SciTech Connect

    White, C.M.; Li, N.C.

    1982-08-01

    The gas chromatographic retention characteristics of a variety of underivatized phenols have been studied by using Superox-20M coated on fused silica. The relative retention times of thes compounds were measured at 160, 150, and 140/sup 0/C in order to determine the effect of operating temperature on relative retention. This information is used to predict relative retention times of phenols for which we had no standards. The linear temperature-programmed retention indexes of the solutes were measured. The retention of phenols on this phase is a function of the compounds vapor pressure, its ability to hydrogen bond with the stationary phase, and the strengths of those hydrogen bonds. These properties are in turn governed by steric, inductive, and resonance effects of the substituents. Linear free-energy relations between the logarithm of the ratio of the activity coefficients of phenol to substituted phenol (calculated from relative retention data) and the chromatographic substituent constant, sigma/sub c/, have been determined for some phenols on Superox-20M. Lastly, it was shown by nuclear magnetic resonance experiments that Superox-20M is apparently a poly(ethylene glycol) (also called a polyoxiran or poly(ethylene oxide)). 5 figures, 3 tables.

  16. Thin layer chromatographic determination of deoxynivalenol in processed grain products.

    PubMed

    Trucksess, M W; Flood, M T; Page, S W

    1986-01-01

    The thin layer chromatographic (TLC) method of Trucksess et al. (J. Assoc. Off. Anal. Chem. (1984) 67, 40-43) was modified for the determination of deoxynivalenol (DON) in high-sugar breakfast cereals, corn syrup, and beer. Celite was added to the substrate before extraction with acetonitrile-water (84 + 16). After filtration through an alumina-charcoal-Celite (0.5 + 0.7 + 0.3) column, the filtrate was evaporated to dryness and redissolved in water, which was passed through an octylsilyl reverse phase column. DON was eluted with anhydrous ethyl ether. The residue remaining after the eluate was evaporated to dryness was dissolved in CHCl3-acetonitrile (4 + 1) and chromatographed on AlCl3-impregnated silica gel TLC plates. The blue fluorescent DON spot was quantitated fluorodensitometrically after the TLC plate was heated at 120 degrees C for 7 min. Recoveries of DON added to breakfast cereals at 100, 200, and 400 ng/g levels and to syrup and beer at 50, 100, and 200 ng/g levels averaged 86%. The limit of determination in these products was about 50 ng/g.

  17. A discontinuous Galerkin method to solve chromatographic models.

    PubMed

    Javeed, Shumaila; Qamar, Shamsul; Seidel-Morgenstern, Andreas; Warnecke, Gerald

    2011-10-07

    This article proposes a discontinuous Galerkin method for solving model equations describing isothermal non-reactive and reactive chromatography. The models contain a system of convection-diffusion-reaction partial differential equations with dominated convective terms. The suggested method has capability to capture sharp discontinuities and narrow peaks of the elution profiles. The accuracy of the method can be improved by introducing additional nodes in the same solution element and, hence, avoids the expansion of mesh stencils normally encountered in the high order finite volume schemes. Thus, the method can be uniformly applied up to boundary cells without loosing accuracy. The method is robust and well suited for large-scale time-dependent simulations of chromatographic processes where accuracy is highly demanding. Several test problems of isothermal non-reactive and reactive chromatographic processes are presented. The results of the current method are validated against flux-limiting finite volume schemes. The numerical results verify the efficiency and accuracy of the investigated method. The proposed scheme gives more resolved solutions than the high resolution finite volume schemes.

  18. Chemical and morphological changes in hydrochars derived from microcrystalline cellulose and investigated by chromatographic, spectroscopic and adsorption techniques.

    PubMed

    Diakité, Mamadou; Paul, Andrea; Jäger, Christian; Pielert, Judith; Mumme, Jan

    2013-12-01

    Hydrothermal carbonization (HTC) can be used for converting the biomass into a carbon-rich material, whose application as a fuel requires higher heating value, whereas soil amendment needs stable carbon. This work was focused on the characterization of hydrochars derived from microcrystalline cellulose. The chars were investigated using elemental analysis, Brunauer-Emmett-Teller technique, nuclear magnetic resonance spectroscopy, Raman, Fourier transform infrared, and electron spin resonance spectroscopy. Severity in temperature between 230 and 270°C with reaction times between 2 and 10 h only affect the carbon content moderately. The results show that aromatization of HTC chars correlates well with temperature, which was further supported by the increase of organic radicals with decreasing g values at higher temperatures. Based on these results, the energetic use of chars favors mild HTC (T<230°C and t≤6 h), while the soil amendement favors serve conditions (T≥230°C, and t>6 h).

  19. Radical-mediated step-growth: Preparation of hybrid polymer monolithic columns with fine control of nanostructural and chromatographic characteristics.

    PubMed

    Alves, Filipa; Nischang, Ivo

    2015-09-18

    chromatographic separations of small molecules across wide ranges of retention factors over at least two orders of magnitude and wide ranges of mobile phase compositions. Such experimental observation is explained by a more homogeneous energetic distribution of partition and adsorption sites. A reference analysis of normalized plate height data at varied retention was performed and set in context with data of state-of-the-art silica- and polymer-based monoliths. This analysis clearly identifies the present materials to display performance behavior clearly located in the domain of derivatized silica-based monoliths.

  20. Statistical learning of peptide retention behavior in chromatographic separations: a new kernel-based approach for computational proteomics

    PubMed Central

    Pfeifer, Nico; Leinenbach, Andreas; Huber, Christian G; Kohlbacher, Oliver

    2007-01-01

    Background High-throughput peptide and protein identification technologies have benefited tremendously from strategies based on tandem mass spectrometry (MS/MS) in combination with database searching algorithms. A major problem with existing methods lies within the significant number of false positive and false negative annotations. So far, standard algorithms for protein identification do not use the information gained from separation processes usually involved in peptide analysis, such as retention time information, which are readily available from chromatographic separation of the sample. Identification can thus be improved by comparing measured retention times to predicted retention times. Current prediction models are derived from a set of measured test analytes but they usually require large amounts of training data. Results We introduce a new kernel function which can be applied in combination with support vector machines to a wide range of computational proteomics problems. We show the performance of this new approach by applying it to the prediction of peptide adsorption/elution behavior in strong anion-exchange solid-phase extraction (SAX-SPE) and ion-pair reversed-phase high-performance liquid chromatography (IP-RP-HPLC). Furthermore, the predicted retention times are used to improve spectrum identifications by a p-value-based filtering approach. The approach was tested on a number of different datasets and shows excellent performance while requiring only very small training sets (about 40 peptides instead of thousands). Using the retention time predictor in our retention time filter improves the fraction of correctly identified peptide mass spectra significantly. Conclusion The proposed kernel function is well-suited for the prediction of chromatographic separation in computational proteomics and requires only a limited amount of training data. The performance of this new method is demonstrated by applying it to peptide retention time prediction in IP

  1. Electrokinetic investigation of surfactant adsorption.

    PubMed

    Bellmann, C; Synytska, A; Caspari, A; Drechsler, A; Grundke, K

    2007-05-15

    Fuerstenau [D.W. Fuerstenau, in: M.L. Hair (Ed.), Dekker, New York, 1971, p. 143] has already discussed the role of hydrocarbon chain of surfactants, the effect of alkyl chain length, chain structure and the pH of the solution on the adsorption process of surfactants. Later Kosmulski [M. Kosmulski, Chemical Properties of Material Surfaces, Surfactant Science Series, vol. 102, Dekker, New York, Basel, 2001] included the effect of surfactant concentration, equilibration time, temperature and electrolyte in his approaches. Certainly, the character of the head groups of the surfactant and the properties of the adsorbent surface are the basis for the adsorption process. Different surfactants and adsorbents cause different adsorption mechanisms described firstly by Rosen [M.J. Rosen, Surfactants and Interfacial Phenomena, second ed., Wiley, New York, 1989]. These adsorption mechanisms and their influencing factors were studied by electrokinetic investigations. Here only changes of the charges at the surfaces could be detected. To control the results of electrokinetic investigations they were compared with results from ellipsometric measurements. In the case of surfactant adsorption the chain length was vitally important. It could be shown by the adsorption of alkyl trimethyl ammonium bromides onto polymer films spin coated at wafer surfaces. The influence of the chain length depending on surface properties of the polymer film was studied. Streaming potential measurements were applied for these investigations. The obtained results enabled us to calculate the molar cohesive free energy per mol of CH2-group in the alkaline chain of the surfactant if all other specific adsorption effects were neglected.

  2. Batch uptake of lysozyme: effect of solution viscosity and mass transfer on adsorption.

    PubMed

    Wright, P R; Muzzio, F J; Glasser, B J

    1998-01-01

    In this study, solid-phase adsorption by macroporous and hyper-diffusive resins was investigated in a batch uptake adsorption system to quantify solid-phase diffusion rates as a function of bulk phase viscosity. The performance of chromatographic resins used for adsorption of proteins is dependent on several factors including solid and liquid-phase diffusivity, boundary layer mass transfer, and intraparticle mass transfer effects. Understanding these effects is critical to process development and optimization of both packed and fluidized bed adsorption systems. The macroporous resin used here was Streamline SP, and the hyper-diffusive resin was S-HyperD LS. Both have been frequently used in fluidized bed adsorption of proteins; however, factors that affect uptake rates of these media are not well quantified. Adsorption isotherms were well represented by an empirical fit of a Langmuir isotherm. Solid-phase diffusion coefficients obtained from simulations were in agreement with other models for macroporous and hyper-diffusive particles. S-HyperD LS in the buffer system had the highest uptake rate, but increased bulk phase viscosity decreased the rate by approximately 50%. Increases in bulk phase viscosity increased film mass transfer effects, and uptake was observed to be a strong function of the film mass transfer coefficient. Uptake by Streamline SP particles was slower than S-HyperD in buffer, due to a greater degree of intraparticle mass transfer resistance. The effect of increased film mass transfer resistance coupled with intraparticle mass transfer resistances at an increased bulk phase viscosity resulted in a decrease of 80% in the uptake rate by Streamline SP relative to S-HyperD.

  3. Adsorption of oxygen on W/100/ - Adsorption kinetics and structure

    NASA Technical Reports Server (NTRS)

    Bauer, E.; Poppa, H.; Viswanath, Y.

    1976-01-01

    The adsorption of oxygen on W(100) single-crystal surfaces is studied by Auger electron spectroscopy (AES), flash desorption, low-energy electron diffraction (LEED), and retarding-field work-function measurements. The AES results reveal stepwise changes in the sticking coefficients in the coverage range 0 to 1 and activated adsorption at higher coverages. Upon room-temperature adsorption, a series of complex LEED patterns is observed. In layers adsorbed at 1050 K and cooled to room temperature, the p(2 x 1) structure is the first ordered structure observed. This structure shows a reversible order-disorder transition between 700 and 1000 K and is characterized by a work function which is lower than that of the clean surface. Heating room-temperature adsorbates changes their structure irreversibly. At temperatures below 750 K, some new structures are observed.

  4. Adsorptive desulfurization by activated alumina.

    PubMed

    Srivastav, Ankur; Srivastava, Vimal Chandra

    2009-10-30

    This study reports usage of commercial grade activated alumina (aluminum oxide) as adsorbent for the removal of sulfur from model oil (dibenthiophene (DBT) dissolved in n-hexane). Bulk density of alumina was found to be 1177.77 kg/m(3). The BET surface area of alumina was found to decrease from 143.6 to 66.4 m(2)/g after the loading of DBT at optimum conditions. The carbon-oxygen functional groups present on the surface of alumina were found to be effective in the adsorption of DBT onto alumina. Optimum adsorbent dose was found to be 20 g/l. The adsorption of DBT on alumina was found to be gradual process, and quasi-equilibrium reached in 24 h. Langmuir isotherm best represented the equilibrium adsorption data. The heat of adsorption and change in entropy for DBT adsorption onto alumina was found to be 19.5 kJ/mol and 139.2 kJ/mol K, respectively.

  5. Reduced protein adsorption by osmolytes.

    PubMed

    Evers, Florian; Steitz, Roland; Tolan, Metin; Czeslik, Claus

    2011-06-07

    Osmolytes are substances that affect osmosis and are used by cells to adapt to environmental stress. Here, we report a neutron reflectivity study on the influence of some osmolytes on protein adsorption at solid-liquid interfaces. Bovine ribonuclease A (RNase) and bovine insulin were used as model proteins adsorbing at a hydrophilic silica and at a hydrophobic polystyrene surface. From the neutron reflectivity data, the adsorbed protein layers were characterized in terms of layer thickness, protein packing density, and adsorbed protein mass in the absence and presence of urea, trehalose, sucrose, and glycerol. All data point to the clear effect of these nonionic cosolvents on the degree of protein adsorption. For example, 1 M sucrose leads to a reduction of the adsorbed amount of RNase by 39% on a silica surface and by 71% on a polystyrene surface. Trehalose was found to exhibit activity similar to that of sucrose. The changes in adsorbed protein mass can be attributed to a decreased packing density of the proteins in the adsorbed layers. Moreover, we investigated insulin adsorption at a hydrophobic surface in the absence and presence of glycerol. The degree of insulin adsorption is decreased by even 80% in the presence of 4 M of glycerol. The results of this study demonstrate that nonionic cosolvents can be used to tune and control nonspecific protein adsorption at aqueous-solid interfaces, which might be relevant for biomedical applications.

  6. A biological oil adsorption filter.

    PubMed

    Pasila, Antti

    2004-12-01

    A new oil adsorption method called adsorption filtration (AF) has been developed. It is a technology where by oil residues can be cleaned from water by running it through a simple filter made from freeze treated, dried, milled and then fragmented plant material. By choosing suitable plants and fragmentation sizes it is possible to produce filters, which pass water but adsorb oil. The aim of this study was to investigate the possibilities of manufacturing oil adsorbing filter materials from reed canary grass (Phalaris arundinacea), flax (Linum usitatissimum L.) or hemp fibre (Cannabis sativa L.). The oil (80 ml) was mixed with de-ionised water (200 ml) and this mixture was filtered through 10 or 20 g adsorption filters. Fine spring harvested hemp fibre (diameter less than 1 mm) and reed canary grass fragments adsorb 2-4 g of oil per gram of adsorption material compared to 1-3 g of water. Adsorption filtration is thus a novel way of gathering spilled oil in shallow coastal waters before the oil reaches the shore.

  7. Metal adsorption on mosses: Toward a universal adsorption model.

    PubMed

    González, A G; Pokrovsky, O S

    2014-02-01

    This study quantifies the adsorption of heavy metals on 4 typical moss species used for environmental monitoring in the moss bag technique. The adsorption of Cu(2+), Cd(2+), Ni(2+), Pb(2+) and Zn(2+) onto Hypnum sp., Sphagnum sp., Pseudoscleropodium purum and Brachytecium rutabulum has been investigated using a batch reactor in a wide range of pH (1.3-11.0) and metal concentrations in solution (1.6μM-3.8mM). A Linear Programming Model (LPM) was applied for the experimental data to derive equilibrium constants and the number of surface binding sites. The surface acid-base titration performed for 4 mosses at a pH range of 3-10 in 0.1M NaNO3 demonstrated that Sphagnum sp. is the most efficient adsorbent as it has the maximal number of proton-binding sites on the surface (0.65mmol g(-1)). The pKa computed for all the moss species suggested the presence of 5 major functional groups: phosphodiester, carboxyl, phosphoryl, amine and polyphenols. The results of pH-edge experiments demonstrated that B. rutabulum exhibits the highest percentage of metal adsorption and has the highest number of available sites for most of the metals studied. However, according to the results of the constant pH "Langmuirian" isotherm, Sphagnum sp. can be considered as the strongest adsorbent, although the relative difference from other mosses is within 20%. The LPM was found to satisfactorily fit the experimental data in the full range of the studied solution parameters. The results of this study demonstrate a rather similar pattern of five metal adsorptions on mosses, both as a function of pH and as a metal concentration, which is further corroborated by similar values of adsorption constants. Therefore, despite the species and geographic differences between the mosses, a universal adsorption edge and constant pH adsorption isotherm can be recommended for 4 studied mosses. The quantitative comparison of metal adsorption with other common natural organic and inorganic materials demonstrates

  8. Doxylamine: a cause for false-positive gas chromatographic assay for phencyclidine.

    PubMed

    Schaldenbrand, J D; McClatchey, K D; Patel, J A; Muilenberg, M J

    1981-01-01

    A 25-year-old white woman ingested an unknown quantity of doxylamine succinate and flurazepam. Urine immunoassay screen (EMIT-dau) was positive for benzodiazopine and negative for phencyclidine. Subsequent gas chromatographic assay of the urine revealed a markedly positive assay for phencyclidine. Doxylamine was ultimately found to be the cause for the false-positive gas chromatographic assay for phencyclidine.

  9. Gas chromatograph-mass spectrometer (GC/MS) system for quantitative analysis of reactive chemical compounds

    DOEpatents

    Grindstaff, Quirinus G.

    1992-01-01

    Described is a new gas chromatograph-mass spectrometer (GC/MS) system and method for quantitative analysis of reactive chemical compounds. All components of such a GC/MS system external to the oven of the gas chromatograph are programmably temperature controlled to operate at a volatilization temperature specific to the compound(s) sought to be separated and measured.

  10. Chromatographic hydrophobicity index: pH profile for polyprotic compounds.

    PubMed

    Fuguet, Elisabet; Ràfols, Clara; Bosch, Elisabeth; Rosés, Martí

    2009-11-06

    The Chromatographic Hydrophobicity Index (CHI) has been measured for several diprotic compounds. In order to model the variation of CHI with pH, a general equation for polyprotic compounds which allows the calculation of CHI for each one of the species has been proposed. Different types of diprotic solutes have been selected: neutral acids, neutral bases, and amphiprotic compounds (non-zwitterionic and zwitterionic). The applicability of the model to these complex polyprotic compounds, its advantages and limitations, as well as the information provided by the fits is discussed. In general, the model fits the experimental behaviour of all kind of solutes very well, obtaining the higher hydrophobicity values for the neutral form of the compounds, except for the zwitterionic phenylalanine. The equation and parameters obtained allow an easy calculation of CHI of the compound at any pH value.

  11. Chromatographic resolution of altered forms of protein kinase C

    SciTech Connect

    Ashendel, C.L.; Minor, P.L.; Baudoin, P.A.; Carlos, M.

    1987-05-01

    Rapid chromatographic resolution of protein kinase C (PKC) in extracts of rat brain on DEAE-cellulose yielded two major peaks of activity. These fractions bound phorbol esters with identical affinity and specificity and had similar ratios of PKC to phorbol ester-binding activities. Chicken egg yolk antibodies raised to PKC in the first fraction reacted with 74 to 76 kilodalton peptides in the second fraction. Chromatography of each fraction on hydroxylapatite yielded similar distributions of three PKC isozymes. Rechromatography of the DEAE-cellulose fractions on DEAE-cellulose confirmed that these forms of PKC were not rapidly interconvertible. Results of experiments in which extracts or fractions were incubated with MgATP and phosphatase inhibitors were consistent with elution of dephospho-PKC in the first fraction while the second fraction contained phospho-PKC. If confirmed, this suggests that a substantial fraction of PKC in rat and mouse tissues exists in the phosphorylated form.

  12. Extraction, chromatographic and mass spectrometric methods for lipid analysis.

    PubMed

    Pati, Sumitra; Nie, Ben; Arnold, Robert D; Cummings, Brian S

    2016-05-01

    Lipids make up a diverse subset of biomolecules that are responsible for mediating a variety of structural and functional properties as well as modulating cellular functions such as trafficking, regulation of membrane proteins and subcellular compartmentalization. In particular, phospholipids are the main constituents of biological membranes and play major roles in cellular processes like transmembrane signaling and structural dynamics. The chemical and structural variety of lipids makes analysis using a single experimental approach quite challenging. Research in the field relies on the use of multiple techniques to detect and quantify components of cellular lipidomes as well as determine structural features and cellular organization. Understanding these features can allow researchers to elucidate the biochemical mechanisms by which lipid-lipid and/or lipid-protein interactions take place within the conditions of study. Herein, we provide an overview of essential methods for the examination of lipids, including extraction methods, chromatographic techniques and approaches for mass spectrometric analysis.

  13. Chromatographic evaluation of the toxicity in fish of pesticides.

    PubMed

    Bermúdez-Saldaña, José María; Escuder-Gilabert, Laura; Medina-Hernández, María José; Villanueva-Camañas, Rosa María; Sagrado, Salvador

    2005-01-05

    Ecotoxicity assessment is essential before placing new chemical substances on the market. An investigation of the use of the chromatographic retention (log k) in biopartitioning micellar chromatography (BMC) as an in vitro approach to evaluate the toxicity in fish of pesticides (acute toxicity levels as pLC(50)) is proposed. A heterogeneous data set of 85 pesticides from six chemical families with available experimental fish toxicity data (ECOTOX database from U.S. Environmental Protection Agency (EPA)) was used. For pesticides exhibiting non-polar narcosis mechanism in fish (non-specific toxicity), more reliable models and precise pLC(50) estimations are obtained from log k (quantitative retention-activity relationships, QRAR) than from log P (quantitative structure-activity relationships, QSAR) or ECOSAR (ECOSAR program from U.S. EPA).

  14. Chromatographic separation of neodymium isotopes by using chemical exchange process.

    PubMed

    Ismail, I M; Ibrahim, M; Aly, H F; Nomura, M; Fujii, Y

    2011-05-20

    The neodymium isotope effects were investigated in Nd-malate ligand exchange system using the highly porous cation exchange resin SQS-6. The temperature of the chromatographic columns was kept constant at 50°C by temperature controlled water passed through the columns jackets. The separation coefficient of neodymium isotopes, ɛ's, was calculated from the isotopic ratios precisely measured by means of an ICP mass spectrometer equipped with nine collectors as ion detectors. The separation coefficient, ɛ×10(5), were calculated and found to be 1.4, 4.8, 5.4, 10.6, 16.8 and 20.2 for (143)Nd, (144)Nd, (145)Nd, (146)Nd, (148)Nd and (150)Nd, respectively.

  15. [Thin-layer chromatographic demonstration of the herbicide zenkor].

    PubMed

    Tsvetkova, Ts; Sergeeva, D; Grigorova, D

    1976-01-01

    Established were the thin-layer chromatography conditions for the demonstration of the herbicide Zenkor as a pure substance and a preparation. Comparative experiments were carried out applying Thomson and Stanley's thin-layer chromatography conditions and the authors' personal ones. Most adequate proved to be the following conditions: sorbent-Kieselgel 60F 254 (Merck); solvent -- chloroform: 1,4-dioxan (9:1); developer -- ultraviolet light (authors' technique). Essential with this method is the preliminary (prior to apply the pure substances on the thin-layer chromatographic plaque) moving of the plaque in the indicated mobile phase (authors' technique). Under these thin-layer chromatography conditions work is made feasible and the method is fast and simple, achieving high sensitivity -- 0.5 mug Zenkor.

  16. Mathematical model for multicomponent separations on the continuous annular chromatograph

    SciTech Connect

    Bratzler, R.L.; Begovich, J.M.

    1980-12-01

    A model for multicomponent separations on ion exchange columns has been adapted for use in studying the performance of the continuous annular chromatograph. The model accurately predicts solute peak positions in the column effluent and qualitatively predicts trends in solute effluent resolution as a function of increasing bandwidth of the solute feed pulse. The major virtues of the model are its simplicity in terms of the calculations involved and the fact that it incorporates the nonlinear solute-resin binding isotherms common in many ion exchange separations. Because dispersion effects are not accounted for in the model, discrepancies exist between the shapes of the effluent peaks predicted by the model and those determined experimentally.

  17. The gas chromatographic resolution of DL-isovaline

    NASA Technical Reports Server (NTRS)

    Flores, J. J.; Bonner, W. A.; Van Dort, M. A.

    1977-01-01

    Isovaline is of cosmological interest because it is one of the 12 non-protein amino acids which have been isolated from the Murchison meteorite, and unlike the other chiral amino acids in this meteorite, it has no alpha-hydrogen at its asymmetric center and hence cannot racemize by the customary alpha-hydrogen-dependent mechanisms which engender racemization in ordinary amino acids. Experiments were conducted in which a .01 M solution of N-TFA-DL-isovalyl-L-leucine isopropyl ester in nitromethane was injected into the capillary column of a gas chromatograph coupled to a digital electronic integrator-recorder. Efflux times and integrated peak area percents are shown next to each diastereometer peak.

  18. RAPID MEASUREMENTS OF NEPTUNIUM OXIDATION STATES USING CHROMATOGRAPHIC RESINS

    SciTech Connect

    Diprete, D; C Diprete, C; Mira Malek, M; Eddie Kyser, E

    2009-03-24

    The Savannah River Site's (SRS) H-Canyon facility uses ceric ammonium nitrate (CAN) to separate impure neptunium (Np) from a high sulfate feed stream. The material is processed using a two-pass solvent extraction purification which relies on CAN to oxidize neptunium to Np(VI) during the first pass prior to extraction. Spectrophotometric oxidation-state analyses normally used to validate successful oxidation to Np(VI) prior to extraction were compromised by this feed stream matrix. Therefore, a rapid chromatographic method to validate successful Np oxidation was developed using Eichrom Industries TRU and TEVA{reg_sign} resins. The method was validated and subsequently transferred to existing operations in the process analytical laboratories.

  19. Gas chromatographic determination of oxalic acid in foods.

    PubMed

    Ohkawa, H

    1985-01-01

    A new quantitative gas chromatographic (GC) method has been developed for the determination of oxalic acid in foods. Solid sample is extracted with water (soluble oxalic acid) or 2N hydrochloric acid (total oxalic acid) at room temperature. An aliquot of sample extract is evaporated to dryness, and the oxalic acid in the residue is methylated with 7% hydrochloric acid-methanol. The reaction mixture is extracted with chloroform, and dimethyl oxalate is quantitated by GC. Recovery of oxalic acid added to liquid samples averaged 100.6%; recoveries from extracts of solid samples were 96.2-99.5 and 97.2-100.1% for water and hydrochloric acid extractions, respectively. Results are shown for determination of oxalic acid in spinach and beverages. The technique is simple, rapid, and accurate, and small samples may be used. The limit of determination is 20 micrograms.

  20. Liquid Chromatographic Determination of Amnesic Shellfish Poison in Mussels

    NASA Astrophysics Data System (ADS)

    Duxbury, Mark

    2000-10-01

    A simple, rapid, high-performance liquid chromatographic experiment suitable for undergraduate students is described for determining amnesic shellfish poison in mussels. The poison itself is an unusual naturally occurring amino acid, domoic acid, that has been found in seafood, particularly shellfish, worldwide. The symptoms of poisoning include amnesia (memory loss), loss of balance, mental confusion, nausea, vomiting, diarrhea, coma, and in extreme cases death. The domoic acid is extracted from homogenized mussel tissue by boiling in water for 5 minutes. The homogenate is cooled and centrifuged, and an aliquot of the supernatant is diluted and analyzed by isocratic HPLC using a C18 column and an acetonitrile-water mobile phase at pH 2.5 with UV detection at 242 nm.

  1. Solubilities in supercritical fluids: the application of chromatographic measurement methods

    SciTech Connect

    Smith, R.D.; Udseth, H.R.; Wright, B.W.; Yonker, C.R.

    1987-01-01

    New methods are described for the measurement of the solubilities of solids in supercritical fluids. These methods utilize instrumentation developed for capillary supercritical fluid chromatography consisting of deactivated, small diameter, fused silica tubing, coupled with detection methods based upon on flame ionization and mass spectrometric detectors. The methods involve (a) direct solubility determination where the fused silica capillary is used as an equilibrium cell, and (b) a pressure of threshold solubility technique which resembles chromatography and uses a programmed pressure increase and sensitive detection to determine the onset of solute migration. Results are also presented which suggest that solubilities can be determined, within certain limitations, from actual chromatographic experiments. The methods are illustrated using aromatic hydrocarbons and complex mycotoxins of the trichothecene group.

  2. Allyl-silica Hybrid Monoliths For Chromatographic Application

    NASA Astrophysics Data System (ADS)

    Guo, Wenjuan

    Column technology continues to be the most investigated topics in the separation world, since the column is the place where the chromatographic separation happens, making it the heart of the separation system. Allyl-silica hybrid monolithic material has been exploited as support material and potential stationary phases for liquid chromatography; the stationary phase anchored to the silica surface by Si-C bond, which is more pH stable than traditional stationary phase. First, nuclear magnetic resonance spectroscopy has been used to study the sol in the synthesis of allyl-silica hybrid monoliths. Allyl-trimethoxysilane (allyl-TrMOS), dimethyldimethoxysilane (DMDMOS) and tetramethoxysilane (TMOS) have been served as co-precursors in the sol-gel synthesis of organo-silica hybrid monolithic columns for liquid chromatography (LC). 29Si nuclear magnetic resonance (NMR) and 1H NMR spectroscopy were employed to monitor reaction profiles for the acid-catalyzed hydrolysis and initial condensation reactions of the individual precursor and the hybrid system. 29Si-NMR has also been used to identify different silane species formed during the reactions. The overall hydrolysis rate has been found to follow the trend DMDMOS > allyl-TrMOS > TMOS, if each precursor is reacted individually (homo-polymerization). Precursors show different hydrolysis rate when reacted together in the hybrid system than they are reacted individually. Cross-condensation products of TMOS and DMDMOS (QD) arise about 10 minutes of initiation of the reaction. The allyl-silica monolithic columns for capillary liquid chromatography can only be prepared in capillaries with 50 im internal diameter with acceptable performance. One of the most prominent problems related to the synthesis of silica monolithic structures is the volume shrinkage. The synthesis of allylfunctionalized silica hybrid monolithic structures has been studied in an attempt to reduce the volume shrinkage during aging, drying and heat treatment

  3. Gas chromatographic determination of sulphur compounds in town gas.

    PubMed

    Hoshika, Y; Iida, Y

    1977-04-11

    The gas chromatographic (GC) determination of the sulphur compounds in town gas (in the Nagoya area) was studied by using a flame-photometric detector (FPD) and the cold-trap method with liquid oxygen. The column packings used were 25% TCEP on Shimalite (AW, DMCS), 25% TCP on Shimalite (AW, DMCS), 10% PPE on Shimalite TPA, Porapak Q and silica gel. The major components identified were carbonyl sulphide, hydrogen sulphide, carbon disulphide, thiophene and tetrahydrothiophene (THT). The identities of thiophene and THT were also confirmed by GC combined with the use of a quadrupole mass spectrometer. The average concentrations and standard deviations of thiophene and THT were 8.8 +/- 1.8and 124 +/- 35 ng per 0.051, respectively. The latter value corresponds to 0.7 ppm, which is relatively high for the concentration of an odorant.

  4. Fatty acids determination in Bronte pistachios by gas chromatographic method.

    PubMed

    Pantano, Licia; Lo Cascio, Giovanni; Alongi, Angelina; Cammilleri, Gaetano; Vella, Antonio; Macaluso, Andrea; Cicero, Nicola; Migliazzo, Aldo; Ferrantelli, Vincenzo

    2016-10-01

    A gas chromatographic with flame ionization detector (GC-MS FID) method for the identification and quantification of fatty acids based on the extraction of lipids and derivatisation of free acids to form methyl esters was developed and validated. The proposed method was evaluated to a number of standard FAs, and Bronte pistachios samples were used for that purpose and to demonstrate the applicability of the proposed method. In this regard, repeatability, mean and standard deviation of the analytical procedure were calculated. The results obtained have demonstrated oleic acid as the main component of Bronte pistachios (72.2%) followed by linoleic acid (13.4%) and showed some differences in composition with respect to Tunisian, Turkish and Iranian pistachios.

  5. Soil chromatographic movement of technetium-99 through selected Minnesota soils

    SciTech Connect

    Balogh, J.C.; Grigal, D.F.

    1980-11-01

    We monitored the movement of technetium-99 through 41 samples of Minnesota soils, using soil column layer chromatography (CLC), a modification of soil thin layer chromatography. Under the aerobic conditions of soil CLC, /sup 99/Tc occurs as the pertechnetate anion. Pertechnetate movement in the soils was characterized by the traditional R/sub f/ chromatographic parameter. Reduced R/sub f/ values were statistically related to elevated levels of soil organic matter. Complexation of /sup 99/Tc, related to soil organic matter, was weak. Elution patterns of /sup 99/Tc in the soil CLC columns were asymmetric, with pertechnetate retardation associated with both hydrodynamic dispersion and weak retention. Pertechnetate was less mobile than was Cl/sup -/ in selected soils by soil CLC.

  6. Improved Chromatographic Separation of Sitagliptin Phosphate and Metformin Hydrochloride

    PubMed Central

    Hendy, Moataz S.

    2015-01-01

    New UPLC method was developed for determination of sitagliptin and metformin using Symmetry C18 column (100 mm × 2.1 mm, 2.2 μm) and isocratic elution (methanol 20%), pH (3.5) as a mobile phase. The ultraviolet detector was operated at 220 nm and the column temperature was 50°C. Linearity parameters were acceptable over the concentration ranges of 2-12 μgml-1 and 5-35 μgml-1 for sitagliptin and metformin, respectively. The variables were premeditated to adjust the chromatographic conditions using design of experiment. The proposed method was proved to be accurate for the quality control of the mentioned drugs in their pharmaceutical dosage form. PMID:26759536

  7. [Advancement of colloidal gold chromatographic technique in screening of ochratoxin A].

    PubMed

    Zhou, Wei-lu; Wang, Yu-ting; Kong, Wei-jun; Yang, Mei-hua; Zhao, Ming; Ou-Yang, Zhen

    2015-08-01

    Ochratoxin A (OTA) is a toxic secondary metabolite mainly produced by Aspergillus and Penicillium species, existing in a variety of foodstuffs and Chinese medicines. OTA is difficult to be detected in practice because of the characteristics such as trace amounts, toxicity, existing in complex matrices. In the numerous detection technologies, colloidal gold chromatographic techniques are highly sensitive, specific, cost-effective and user-friendly, and are being used increasingly for OTA screening. Recently, with the development of aptamer technology and its application in chromatographic technique, a newly colloidal gold aptamer chromatographic technique has been developed. This review elaborates the structures and principles of both traditional and newly colloidal gold chromatographic techniques, focuses on newly colloidal gold aptamer chromatographic technique, summarizes and compares their use in rapid detection of OTA. Finally, in order to provide a reference for better research of related work, the development trends of this novel technique are prospected.

  8. Chemical characterization of Brickellia cavanillesii (Asteraceae) using gas chromatographic methods.

    PubMed

    Eshiet, Etetor R; Zhu, Jinqiu; Anderson, Todd A; Smith, Ernest E

    2014-03-01

    A methanol extract of lyophilized Brickellia cavanillesii was quantitatively analyzed using gas chromatographic (GC) techniques. The chromatographic methods employed were (i) GC-flame ionization detector (GC-FID), (ii) GC-mass spectrometry (GC-MS), and (iii) purge and trap GC-MS (P&T GC-MS). Thirteen compounds were identified with a quality match of 90% and above using GC-MS. The compounds were (1) Cyclohexene, 6-ethenyl-6-methyl-1-(1-methylethyl)-3-(1-methylethylidene)-, (S)-; (2) Bicylo (2.2.1) heptan-2-one, 1, 7, 7-trimethyl-(1S, 4S)-; (3) Phenol, 2-methoxy-4-(1-propenyl)-; (4) Benzene, 1-(1, 5-dimethyl-4-hexenyl)-4-methyl-; (5) Naphthalene, 1, 2, 3, 5, 6, 8a-hexahydro4, 7-dimethyl-1-1-(1-methylethyl)-, (1S-cis)-; (6) Phenol, 2-methoxy-; (7) Benzaldehyde, 3-hydroxy-4-methoxy-; (8) 11, 13-Eicosadienoic acid, methyl ester; (9) 2-Furancarboxaldehyde, 5-methyl-; (10) Maltol; (11) Phenol; (12) Hydroquinone; (13) 1H-Indene, 1-ethylideneoctahydro-7a-methyl-, (1E, 3a.alpha, 7a.beta.). Other compounds (14) 3-methyl butanal; (15) (D)-Limonene; (16) 1-methyl-4-(1-methyl ethyl) benzene; (17) Butanoic acid methyl ester; (18) 2-methyl propanal; (19) 2-butanone; (20) 2-pentanone; and (21) 2-methyl butane were also identified when P&T GC-MS was performed. Of the 21 compounds identified, 12 were validated using chemical standards. The identified compounds were found to be terpenes, derivatives of terpenes, esters, ketones, aldehydes, and phenol-derived aromatic compounds; these are the primary constituents of the essential oils of many plants and flowers.

  9. Chemical characterization of Brickellia cavanillesii (Asteraceae) using gas chromatographic methods

    PubMed Central

    Eshiet, Etetor R; Zhu, Jinqiu; Anderson, Todd A; Smith, Ernest E

    2014-01-01

    A methanol extract of lyophilized Brickellia cavanillesii was quantitatively analyzed using gas chromatographic (GC) techniques. The chromatographic methods employed were (i) GC-flame ionization detector (GC-FID), (ii) GC-mass spectrometry (GC-MS), and (iii) purge and trap GC-MS (P&T GC-MS). Thirteen compounds were identified with a quality match of 90% and above using GC-MS. The compounds were (1) Cyclohexene, 6-ethenyl-6-methyl-1-(1-methylethyl)-3-(1-methylethylidene)-, (S)-; (2) Bicylo (2.2.1) heptan-2-one, 1, 7, 7-trimethyl-(1S, 4S)-; (3) Phenol, 2-methoxy-4-(1-propenyl)-; (4) Benzene, 1-(1, 5-dimethyl-4-hexenyl)-4-methyl-; (5) Naphthalene, 1, 2, 3, 5, 6, 8a-hexahydro4, 7-dimethyl-1-1-(1-methylethyl)-, (1S-cis)-; (6) Phenol, 2-methoxy-; (7) Benzaldehyde, 3-hydroxy-4-methoxy-; (8) 11, 13-Eicosadienoic acid, methyl ester; (9) 2-Furancarboxaldehyde, 5-methyl-; (10) Maltol; (11) Phenol; (12) Hydroquinone; (13) 1H-Indene, 1-ethylideneoctahydro-7a-methyl-, (1E, 3a.alpha, 7a.beta.). Other compounds (14) 3-methyl butanal; (15) (D)-Limonene; (16) 1-methyl-4-(1-methyl ethyl) benzene; (17) Butanoic acid methyl ester; (18) 2-methyl propanal; (19) 2-butanone; (20) 2-pentanone; and (21) 2-methyl butane were also identified when P&T GC-MS was performed. Of the 21 compounds identified, 12 were validated using chemical standards. The identified compounds were found to be terpenes, derivatives of terpenes, esters, ketones, aldehydes, and phenol-derived aromatic compounds; these are the primary constituents of the essential oils of many plants and flowers. PMID:24804069

  10. Understanding and design of existing and future chromatographic support formats.

    PubMed

    Billen, J; Desmet, G

    2007-10-19

    The present contribution reviews the use of alternative support formats as a means to surpass the chromatographic performance of the packed bed of spheres. First, a number of idealized structures are considered to obtain a general insight in how the performance of a chromatographic support depends on its shape and size, using the isocratic peak-capacity generation speed as the main performance indicator. Using this criterion, it is found that the packing density or, equivalently, the external porosity, is the most important of all geometrical shape factors. Depending on whether the sample consists of weakly or strongly retained components, the optimal external porosity can be expected to vary between 60% and a value near 100%. The optimal exploitation of a high external porosity, however, also requires overall shrinkage of the domain size, towards and into the sub-micron range. With the current fabrication technologies, this requirement seems difficult to achieve. In the presence of a lower limit on the characteristic support size, each range of desired plate numbers or peak capacities has its own optimal external porosity, ranging from a very low value (high packing density) for high speed, small peak capacity applications, to very high external porosities (low packing density) for applications requiring a very large peak capacity. Subsequently, the obtained theoretical insights are used to review and discuss the past and current research on alternative support formats. Finally, a number of emerging micro- and nano-fabrication technologies are introduced and their potential for the future production of supports with improved shape and homogeneity is discussed.

  11. Adsorption isotherms of charged nanoparticles.

    PubMed

    Dos Santos, Alexandre P; Bakhshandeh, Amin; Diehl, Alexandre; Levin, Yan

    2016-10-19

    We present theory and simulations which allow us to quantitatively calculate the amount of surface adsorption excess of charged nanoparticles onto a charged surface. The theory is very accurate for weakly charged nanoparticles and can be used at physiological concentrations of salt. We have also developed an efficient simulation algorithm which can be used for dilute suspensions of nanoparticles of any charge, even at very large salt concentrations. With the help of the new simulation method, we are able to efficiently calculate the adsorption isotherms of highly charged nanoparticles in suspensions containing multivalent ions, for which there are no accurate theoretical methods available.

  12. Thermodynamic features of dioxins' adsorption.

    PubMed

    Prisciandaro, Marina; Piemonte, Vincenzo; di Celso, Giuseppe Mazziotti; Ronconi, Silvia; Capocelli, Mauro

    2017-02-15

    In this paper, the six more poisonous species among all congeners of dioxin group are taken into account, and the P-T diagram for each of them is developed. Starting from the knowledge of vapour tensions and thermodynamic parameters, the theoretical adsorption isotherms are calculated according to the Langmuir's model. In particular, the Langmuir isotherm parameters (K and wmax) have been validated through the estimation of the adsorption heat (ΔHads), which varies in the range 20-24kJ/mol, in agreement with literature values. This result will allow to put the thermodynamical basis for a rational design of different process units devoted to dioxins removal.

  13. Counterion release and electrostatic adsorption

    PubMed

    Sens; Joanny

    2000-05-22

    The effective charge of a rigid polyelectrolyte (PE) approaching an oppositely charged surface is studied. The cases of a weak (annealed) and strongly charged PE with condensed counterions (such as DNA) are discussed. In the most interesting case of the adsorption onto a substrate of low dielectric constant (such as a lipid membrane or a mica sheet) the condensed counterions are not always released as the PE approaches the substrate, because of the major importance of the image-charge effect. For the adsorption onto a surface with freely moving charges, the image-charge effect becomes less important and full release is often expected.

  14. Gas chromatographic determination of polycyclic aromatic hydrocarbons in water and smoked rice samples after solid-phase microextraction using multiwalled carbon nanotube loaded hollow fiber.

    PubMed

    Matin, Amir Abbas; Biparva, Pourya; Gheshlaghi, Mohammad

    2014-12-29

    A novel solid-phase microextraction fiber was prepared based on multiwalled carbon nanotubes (MWCNTs) loaded on hollow fiber membrane pores. Stainless steel wire was used as unbreakable support. The major advantages of the proposed fiber are its (a) high reproducibility due to the uniform structure of the hollow fiber membranes, (b) high extraction capacity related to the porous structure of the hollow fiber and outstanding adsorptive characteristics of MWCNTs. The proposed fiber was applied for the microextraction of five representative polycyclic aromatic hydrocarbons (PAHs) from aqueous media (river and hubble-bubble water) and smoked rice samples followed by gas chromatographic determination. Analytical merits of the method, including high correlation coefficients [(0.9963-0.9992) and (0.9982-0.9999)] and low detection limits [(9.0-13.0ngL(-1)) and (40.0-150.0ngkg(-1))] for water and rice samples, respectively, made the proposed method suitable for the ultra-trace determination of PAHs.

  15. Modeling experimental stable isotope results from CO2 adsorption and diffusion experiments

    NASA Astrophysics Data System (ADS)

    Larson, T. E.

    2012-12-01

    Transport of carbon dioxide through porous media can be affected by diffusion, advection and adsorption processes. Developing new tools to understand which of these processes dominates migration of CO2 or other gases in the subsurface is important to a wide range of applications including CO2 storage. Whereas advection rates are not affected by isotope substitution in CO2, adsorption and diffusion constants are. For example, differences in the binary diffusion constant calculated between C12O2-He and C13O2-He results in a carbon isotope fractionation whereby the front of the chromatographic peak is enriched in carbon-12 and the tail of the peak is enriched in carbon-13. Interestingly, adsorption is shown to have an opposite, apparent inverse affect whereby the lighter isotopologues of CO2 are preferentially retained by the chromatographic column and the heavier isotopologues are eluted first. This apparent inverse chromatographic effect has been ascribed to Van der Waals dispersion forces. Smaller molar volumes of the heavier isotopologues resulting from increased bond strength (shorter bond length) effectively decreases Van der Waals forces in heavier isotopologues compared to lighter isotopologues. Here we discuss the possible application of stable isotope values measured across chromatographic peaks to differentiate diffusion-dominated from adsorption-dominated transport processes for CO2. Separate 1-dimensional flow-through columns were packed with quartz and illite, and one remained empty. Dry helium was used as a carrier gas. Constant flow rate, temperature and column pressure were maintained. After background CO2 concentrations were minimized and constant, a sustained pulse of CO2 was injected at the head of the column and the effluent was sampled at 4 minute intervals for CO2 concentration, and carbon and oxygen isotope ratios. The quartz-sand packed and empty columns resulted in similar trends in concentration and isotope ratios whereby CO2 concentrations

  16. Synthesis of metronidazole-imprinted molecularly imprinted polymers by distillation precipitation polymerization and their use as a solid-phase adsorbent and chromatographic filler.

    PubMed

    Liu, Jiang; Zhang, Lu; Li Han Song, Le; Liu, Yuan; Tang, Hui; Li, Yingchun

    2015-04-01

    Metronidazole-imprinted polymers with superior recognition properties were prepared by a novel strategy called distillation-precipitation polymerization. The as-obtained polymers were characterized by Fourier-transform infrared spectroscopy, laser particle size determination and scanning electron microscopy, and their binding performances were evaluated in detail by static, kinetic and dynamic rebinding tests, and Scatchard analysis. The results showed that when the fraction of the monomers was 5 vol% in the whole reaction system, the prepared polymers afforded good morphology, monodispersity, and high adsorption capacity and excellent selectivity to the target molecule, metronidazole. The optimal binding performance is 12.41 mg/g for metronidazole just before leakage occurred and 38.51 mg/g at saturation in dynamic rebinding tests. Metronidazole-imprinted polymers were further applied as packing agents in solid-phase extraction and as chromatographic filler, both of which served for the detection of metronidazole in fish tissue. The results illustrated the recoveries of spiked samples ranged from 82.97 to 87.83% by using molecularly imprinted solid-phase extraction combined with a C18 commercial column and 93.7 to 101.2% by directly using the polymer-packed chromatographic column. The relative standard deviation of both methods was less than 6%.

  17. Adsorption of Organics from Domestic Water Supplies.

    ERIC Educational Resources Information Center

    McGuire, Michael J.; Suffet, Irwin H.

    1978-01-01

    This article discusses the current state of the art of organics removal by adsorption. Various theoretical explanations of the adsorption process are given, along with practical results from laboratory, pilot-scale, and full-scale applications. (CS)

  18. CONTAMINANT ADSORPTION AND OXIDATION VIA FENTON REACTION

    EPA Science Inventory

    A ground water treatment process is proposed involving two cgemical processes: adsorption and oxidation. Adsorption of an organic compound onto granulated activated carbon (GAC) containing iron conveniently results in immobilizing and concentrating contaminants from the ground w...

  19. Improving the productivity of a multidimensional chromatographic preparative system by collecting pure chemicals after each of three chromatographic dimensions.

    PubMed

    Sciarrone, Danilo; Pantò, Sebastiano; Donato, Paola; Mondello, Luigi

    2016-12-02

    The enhanced sample collection capability of a heart-cutting three-dimensional GC-prep system is reported. In its original configuration, a highly pure component can be usually collected after the last (3D) column outlet by means of a dedicated preparative station. The latter is located after the last chromatographic column, and this poses the requirement for multiple heart cuts even for those components showing satisfactory degree of purity after the first (or second) separation dimension. The feasibility to collect pure components after each chromatographic dimension is here described, employing a three-dimension MDGC system equipped with high-temperature valves, located inside the first and second GC ovens, with the aim to improve the productivity of the collection procedure. In addition to a commercial preparative collector located at the 3D outlet, two laboratory-made collection systems were applied in the first and second dimension, reached by the effluent to be collected trough a high-temperature valve switching the heart-cut fraction between either the detector (FID), or the collector. Highly pure sesquiterpene components were collected, namely: patchouli alcohol after the first column [poly(5% diphenyl/95% dimethylsiloxane)], α-bulnesene after a second column coated with high molecular weight polyethylene glycol, and α-guaiene after an ionic-liquid based column (SLB-IL60), used as the third dimension. Purity levels ranging from 85 to 95% were achieved with an average collection recovery of 90% (n=5). The following average amounts were collected per run: 160μg for α-guaiene, 295μg for α-bulnesene, and 496μg for patchouli alcohol.

  20. Multivariate curve resolution based chromatographic peak alignment combined with parallel factor analysis to exploit second-order advantage in complex chromatographic measurements.

    PubMed

    Parastar, Hadi; Akvan, Nadia

    2014-03-13

    In the present contribution, a new combination of multivariate curve resolution-correlation optimized warping (MCR-COW) with trilinear parallel factor analysis (PARAFAC) is developed to exploit second-order advantage in complex chromatographic measurements. In MCR-COW, the complexity of the chromatographic data is reduced by arranging the data in a column-wise augmented matrix, analyzing using MCR bilinear model and aligning the resolved elution profiles using COW in a component-wise manner. The aligned chromatographic data is then decomposed using trilinear model of PARAFAC in order to exploit pure chromatographic and spectroscopic information. The performance of this strategy is evaluated using simulated and real high-performance liquid chromatography-diode array detection (HPLC-DAD) datasets. The obtained results showed that the MCR-COW can efficiently correct elution time shifts of target compounds that are completely overlapped by coeluted interferences in complex chromatographic data. In addition, the PARAFAC analysis of aligned chromatographic data has the advantage of unique decomposition of overlapped chromatographic peaks to identify and quantify the target compounds in the presence of interferences. Finally, to confirm the reliability of the proposed strategy, the performance of the MCR-COW-PARAFAC is compared with the frequently used methods of PARAFAC, COW-PARAFAC, multivariate curve resolution-alternating least squares (MCR-ALS), and MCR-COW-MCR. In general, in most of the cases the MCR-COW-PARAFAC showed an improvement in terms of lack of fit (LOF), relative error (RE) and spectral correlation coefficients in comparison to the PARAFAC, COW-PARAFAC, MCR-ALS and MCR-COW-MCR results.

  1. Modeling of the simulated countercurrent moving-bed chromatographic reactor used for the oxidative coupling of methane

    SciTech Connect

    Tonkovich, A.L.Y.; Carr, R.W.

    1994-09-01

    The oxidative coupling reaction of methane (OCM) is a potential industrial reaction for the efficient production of ethylene. Replacement of current technologies requires significant product yield improvements. An experimental novel reactor design, the modified simulated countercurrent moving-bed chromatographic reactor (SCMCR), has reported improved ethane and ethylene product yields over other reported values. An understanding of the reactor operation is aided by concurrent mathematical modeling. The model mimics the exact experimental reactor configuration. Four sections are used; each section contains a reaction column and two separation columns connected in series. The feed is switched from section to section at discrete intervals. Reaction occurs in the first column and is followed by product and reactant separation in the ensuing section columns. Langmuir adsorption isotherms are used. The model does not incorporate the realistic and complex kinetics rising, from the OCM, rather a simplified reaction term is used to qualitatively gain insight into the operation of the modified SCMCR. A unimolecular reaction network is used in the model. The rate constants are set to permit a small fractional conversion, 5% per pass, at the concentrations during the first cycle. Similarly to the experimental reactor, the model adds a make-up feed (defined as percentage of the original feed, where excess methane is fed during the first cycle of the experimental reactor) to augment lost reactants.

  2. Systematic interpolation method predicts protein chromatographic elution from batch isotherm data without a detailed mechanistic isotherm model.

    PubMed

    Creasy, Arch; Barker, Gregory; Yao, Yan; Carta, Giorgio

    2015-09-01

    Predicting protein elution for overloaded ion exchange columns requires models capable of describing protein binding over broad ranges of protein and salt concentrations. Although approximate mechanistic models are available, they do not always have the accuracy needed for precise predictions. The aim of this work is to develop a method to predict protein chromatographic behavior from batch isotherm data without relying on a mechanistic model. The method uses a systematic empirical interpolation (EI) scheme coupled with a lumped kinetic model with rate parameters determined from HETP measurements for non-binding conditions, to numerically predict the column behavior. For two experimental systems considered in this work, predictions based on the EI scheme are in excellent agreement with experimental elution profiles under highly overloaded conditions without using any adjustable parameters. A qualitative study of the sensitivity of predicting protein elution profiles to the precision, granularity, and extent of the batch adsorption data shows that the EI scheme is relatively insensitive to the properties of the dataset used, requiring only that the experimental ranges of protein and salt concentrations overlap those under which the protein actually elutes from the column and possess a ± 10% measurement precision.

  3. Development and validation of a hydrophilic interaction liquid chromatographic method for determination of aromatic amines in environmental water.

    PubMed

    Li, Ruiping; Zhang, Yi; Lee, Charles C; Lu, Rongrong; Huang, Yingping

    2010-03-12

    A simple, precise, and accurate hydrophilic interaction liquid chromatographic (HILIC) method has been developed for the determination of five aromatic amines in environmental water samples. Chromatography was carried out on a bare silica column, using a mixture of acetonitrile and a buffer of NaH(2)PO(4)-H(3)PO(4) (pH 1.5, containing 10mM NaH(2)PO(4)) (85:15, v/v) as a mobile phase at a flow rate of 1 mL min(-1). Aromatic amines were detected by UV absorbance at 254 nm. The linear range of amines was good (r(2)>0.998) and limit of detection (LOD) within 0.02-0.2 mg L(-1) (S/N=3). The retention mechanism for the analytes under the optimum conditions was determined to be a combination of adsorption, partition and ionic interactions. The proposed method was applied to the environmental water samples. Aromatic amines were isolated from aqueous samples using solid-phase extraction (SPE) with Oasis HLB cartridges. Recoveries of greater than 75% with precision (RSD) less than 12% were obtained at amine concentrations of 5-50 microg L(-1) from 100mL river water and influents from a wastewater treatment plant (WWTP). The present HILIC technique proved to be a viable method for the analysis of aromatic amines in the environmental water samples.

  4. ADSORPTION OF SURFACTANT ON CLAYS

    EPA Science Inventory

    Surfactants used to enhance remediation of soils by soil washing are often lost in the process. Neither the amount nor the cause of this loss is known. It is assumed that clays present in the soil are responsible for the loss of the surfactant. In this papere, adsorption prope...

  5. Engineering and Design: Adsorption Design Guide

    DTIC Science & Technology

    2001-03-01

    adsorptive media addressed in- clude granular activated carbon (GAC) and other alternative adsorption carbon media, such as powdered activated carbon (PAC... Adsorption Media. a. Activated Carbon . Activated carbon can be manufactured from carbonaceous material, in- cluding coal (bituminous, subbituminous...information contained in Corps of Engineers Guide Specification 11225: Downflow Liquid Granular Activated Carbon

  6. Chromatographic and computational assessment of lipophilicity using sum of ranking differences and generalized pair-correlation.

    PubMed

    Andrić, Filip; Héberger, Károly

    2015-02-06

    Lipophilicity (logP) represents one of the most studied and most frequently used fundamental physicochemical properties. At present there are several possibilities for its quantitative expression and many of them stems from chromatographic experiments. Numerous attempts have been made to compare different computational methods, chromatographic methods vs. computational approaches, as well as chromatographic methods and direct shake-flask procedure without definite results or these findings are not accepted generally. In the present work numerous chromatographically derived lipophilicity measures in combination with diverse computational methods were ranked and clustered using the novel variable discrimination and ranking approaches based on the sum of ranking differences and the generalized pair correlation method. Available literature logP data measured on HILIC, and classical reversed-phase combining different classes of compounds have been compared with most frequently used multivariate data analysis techniques (principal component and hierarchical cluster analysis) as well as with the conclusions in the original sources. Chromatographic lipophilicity measures obtained under typical reversed-phase conditions outperform the majority of computationally estimated logPs. Oppositely, in the case of HILIC none of the many proposed chromatographic indices overcomes any of the computationally assessed logPs. Only two of them (logkmin and kmin) may be selected as recommended chromatographic lipophilicity measures. Both ranking approaches, sum of ranking differences and generalized pair correlation method, although based on different backgrounds, provides highly similar variable ordering and grouping leading to the same conclusions.

  7. Chromatographic Separation and NMR An Integrated Approach in Pharmaceutical Development.

    PubMed

    Gonnella, Nina C

    2012-01-01

    Over the past 10 years, major improvements in the performance of LC-NMR have been realized. The addition of postcolumn SPE, advances in probe technology including cryogenic probes and microcoil probes, improved solvent suppression pulse sequences, and shielded magnets with better homogeneity have all contributed to rapid advancements in this technology. Application of LC-NMR to problems in pharmaceutical development has had a major impact on structure elucidation studies. LC-NMR has been successfully applied to determine the structures of degradation products, impurities, mixtures of compounds, and metabolites. Use of stop flow techniques with LC-NMR experiments has been a critical means of identifying unstable compounds and studying conformational kinetics. The integration of SPE as an intermediate step between the LC unit and the NMR spectrometer has vastly improved the power of the hyphenated technique in trace analysis applications. Online postcolumn enrichment of chromatographic peaks by SPE dramatically reduces the NMR acquisition times by allowing repeated injections to be trapped onto the same cartridge or different cartridges. Because protonated solvents can be easily removed with a drying procedure, solvents and buffers may be freely chosen for maximizing chromatographic separation without compromising NMR spectral quality. The compound of interest may then be eluted from an SPE cartridge using deuterated organic solvent, which helps to reduce dynamic range issues. When combined with cryogenically cooled microcapillary probes, the sensitivity of the NMR signal increases about 10-fold over conventional room temperature probes, enabling full structure characterization at the microgram level. Heteronuclear experiments with concentrations previously only possible in a limited number of cases have now become standard experiments. The availability of HSQC and HMBC experiments and microcoil/cryogenic technology opens the possibility of using LC-(SPE) NMR for the

  8. The Huygens Gas Chromatograph Mass Spectrometer Investigation Of Titan

    NASA Astrophysics Data System (ADS)

    Atreya, Sushil; Harpold, Dan; Owen, Tobias

    2015-04-01

    A decade ago, on 14 January 2005, the Huygens probe of the Cassini-Huygens mission descended through the smog filled atmosphere of Titan and landed on the surface, revealing for the first time the extraordinary nature of Saturn's largest moon. One of the six payload instruments, the gas chromatograph mass spectrometer (GCMS), was crucial for measuring the composition of the atmosphere and the surface of Titan [1,2]. Most of the GCMS findings were "firsts", including the first direct identification of molecular nitrogen as the bulk constituent of the atmosphere, first vertical profile of Titan's second most abundant volatile, methane, first determination of primordial and radiogenic argon, first quantification of a number of stable gas isotopes, and the first measurements of the make-up of Titan's surface. These data are key to understanding why Titan is so unique amongst planetary moons in possessing a massive atmosphere [3], how Titan maintains a cycle of methane complete with surface reservoirs, evaporation and condensation like the hydrological cycle on earth [3,4,5], and what is responsible for the photochemical smog on Titan that plays a central role in the very existence of an atmosphere on Titan [3]. This presentation will discuss the GCMS investigation and how it helped shape our current view of Titan. [website for downloading pdf's of relevant papers: www.umich.edu/~atreya] [1] Niemann, H. B. et al., The abundances of constituents of Titan's atmosphere from the GCMS instrument on the Huygens probe, Nature 438, 779-784, 2005. [2] Niemann, H. B. et al., The composition of Titan's lower atmosphere and simple surface volatiles as measured by the Cassini-Huygens probe gas chromatograph mass spectrometer experiment, J. Geophys. Res. (Planets) 115, 12006, 2010. [3] Atreya S. K., R. D. Lorenz and J. H. Waite, Volatile origin and cycles: Nitrogen and methane, in Titan from Cassini-Huygens, R. H. Brown, J. P. Lebreton and J. Waite, (eds.), Springer Dordrecht

  9. Protein adsorption to poly(ethylenimine)-modified Sepharose FF: V. Complicated effects of counterions.

    PubMed

    Liu, Na; Yu, Linling; Sun, Yan

    2015-07-24

    results indicate that protein adsorption and chromatographic performance with PEI-Sepharose can be improved by proper counterions. For the four counterions tested, SO4(2-) was the most favorable for providing the best adsorption and elution outcomes with FF-PEI-L680.

  10. Chromatographic separation and concentration of quercetin and (+)-catechin using mesoporous composites based on MCM-41

    NASA Astrophysics Data System (ADS)

    Karpov, S. I.; Belanova, N. A.; Korabel'nikova, E. O.; Nedosekina, I. V.; Roessner, F.; Selemenev, V. F.

    2015-05-01

    Data on chromatographic separation of quercetin and (+)-catechin-flavonoids with similar physicochemical (including sorption) properties—are presented. The highest efficiency of chromatographic process at high sorption capacity of the material with respect to quercetin and slightly lower capacity for (+)-catechin were observed when silylated composites of ordered MCM-41 type materials were used. The application of acetonitrile as a solvent increased the sorption capacity of the material and can be recommended for separation of related polyphenol substances and their determination using ordered MCM-41 modified with trimethylchlorosilane as a stationary phase in a chromatographic column.

  11. Considerations on the temperature dependence of the gas-liquid chromatographic retention.

    PubMed

    González, Francisco Rex

    2002-01-04

    A discussion on the temperature dependence of the partition coefficient K is developed. This discussion embraces topics such as the limitations of conventional thermodynamic approaches followed in the chromatographic literature, qualitative theoretical notions arising from molecular thermodynamics and the experimental information that is accessible through modern capillary gas chromatography. It is shown that the heat capacity difference of solute transfer for flexible molecules has at least one maximum in the chromatographic range of temperature. As a consequence, a great amount of experimental data is required for a correct thermodynamic interpretation of the chromatographic retention.

  12. Phosphate adsorption on lanthanum loaded biochar.

    PubMed

    Wang, Zhanghong; Shen, Dekui; Shen, Fei; Li, Tianyu

    2016-05-01

    To attain a low-cost and high-efficient phosphate adsorbent, lanthanum (La) loaded biochar (La-BC) prepared by a chemical precipitation method was developed. La-BC and its pristine biochar (CK-BC) were comparatively characterized using zeta potential, BET surface area, scanning electron microscopy/energy dispersive spectrometer (SEM-EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FT-IR). The adsorption ability and the mechanisms during adsorption process for the La-BC samples were also investigated. La loaded on the surface of biochar can be termed as La-composites (such as LaOOH, LaONO3 and La(OH)3), leading to the decrease of negative charge and surface area of biochar. La-BC exhibited the high adsorption capacity to phosphate compared to CK-BC. Adsorption isotherm and adsorption kinetic studies showed that the Langmuir isotherm and second order model could well describe the adsorption process of La-BC, indicating that the adsorption was dominated by a homogeneous and chemical process. The calculated maximum adsorption capacity was as high as 46.37 mg g(-1) (computed in P). Thermodynamic analysis revealed that the adsorption was spontaneous and endothermic. SEM, XRD, XPS and FT-IR analysis suggested that the multi-adsorption mechanisms including precipitation, ligand exchange and complexation interactions can be evidenced during the phosphate adsorption process by La-composites in La-BC.

  13. Adsorption of organic chemicals in soils.

    PubMed Central

    Calvet, R

    1989-01-01

    This paper presents a review on adsorption of organic chemicals on soils sediments and their constituents. The first part of this review deals with adsorption from gas and liquid phases and gives a discussion on the physical meaning of the shape of adsorption isotherms. Results show that no general rules can be proposed to describe univocally the relation between the shape of isotherms and the nature of adsorbate-adsorbent system. Kinetics of adsorption is discussed through the description of various models. Theoretical developments exist both for the thermodynamics and the kinetics of adsorption, but there is a strong need for experimental results. Possible adsorption mechanisms are ion exchange, interaction with metallic cations, hydrogen bonds, charge transfers, and London-van der Waals dispersion forces/hydrophobic effect. However, direct proofs of a given mechanism are rare. Several factors influence adsorption behavior. Electronic structure of adsorbed molecules, properties of adsorbents, and characteristics of the liquid phase are discussed in relation to adsorption. Such properties as water solubility, organic carbon content of adsorbing materials, and the composition of the liquid phase are particularly important. Evaluation of adsorption can be obtained through either laboratory measurements or use of several correlations. Adsorption measurements must be interpreted, taking into account treatment of adsorbent materials, experimental conditions, and secondary phenomena such as degradations. Correlations between adsorption coefficients and water-octanol partition coefficient or water solubility are numerous. They may be useful tools for prediction purposes. Relations with transport, bioavailability, and degradation are described. PMID:2695323

  14. Micro-miniature gas chromatograph column disposed in silicon wafers

    DOEpatents

    Yu, Conrad M.

    2000-01-01

    A micro-miniature gas chromatograph column is fabricated by forming matching halves of a circular cross-section spiral microcapillary in two silicon wafers and then bonding the two wafers together using visual or physical alignment methods. Heating wires are deposited on the outside surfaces of each wafer in a spiral or serpentine pattern large enough in area to cover the whole microcapillary area inside the joined wafers. The visual alignment method includes etching through an alignment window in one wafer and a precision-matching alignment target in the other wafer. The two wafers are then bonded together using the window and target. The physical alignment methods include etching through vertical alignment holes in both wafers and then using pins or posts through corresponding vertical alignment holes to force precision alignment during bonding. The pins or posts may be withdrawn after curing of the bond. Once the wafers are bonded together, a solid phase of very pure silicone is injected in a solution of very pure chloroform into one end of the microcapillary. The chloroform lowers the viscosity of the silicone enough that a high pressure hypodermic needle with a thumbscrew plunger can force the solution into the whole length of the spiral microcapillary. The chloroform is then evaporated out slowly to leave the silicone behind in a deposit.

  15. Authenticity analysis of pear juice employing chromatographic fingerprinting.

    PubMed

    Willems, Jamie L; Low, Nicholas H

    2014-12-03

    Pear juice is predominately composed of carbohydrates/polyols (>95% of the total soluble solids), making it susceptible to adulteration by the addition of less expensive commercial sweeteners. In this research, the major carbohydrate and polyol (fructose, glucose, sucrose, and sorbitol) content of 32 pure pear juices representing five world producing regions and three years of production was determined. Additionally, methods employing oligosaccharide profiling to detect the debasing of these samples with four commercial sweeteners (HFCS 55 and 90, TIS, and HIS) were developed using capillary gas chromatography with flame ionization detection (CGC-FID) and high-performance liquid chromatography with pulsed amperometric detection (HPAE-PAD). Detection limits for the four commercial sweeteners ranged from 0.5 to 5.0% (v/v). In addition, the developed CGC-FID method could be used to (a) detect the addition of pear to apple juice via arbutin detection and (b) determine if a pear juice was produced using enzymatic liquefaction via the presence of O-β-d-glucopyranosyl-(1→4)-d-glucopyranose (cellobiose), all within a single chromatographic analysis.

  16. Liquid chromatographic determination of progestogens in animal fat.

    PubMed

    Andresen, M T; Fesser, A C

    1996-01-01

    A liquid chromatographic method was developed for determination of 3 progestogens-melengestrol acetate, megestrol acetate, and chlormadinone acetate-found in edible tissue at concentrations between 10 and 1000 ppb. These progestogens are commonly used as feed additives to control herd estrus and to improve feed efficiency. Rendered fat was extracted with acetonitrile, washed with hexane, and dried. The remaining lipids were saponified with sodium hydroxide and precipitated with magnesium chloride. The progestogens were extracted from the basic solution with hexane, dried, and cleaned up on a cyanopropyl solid-phase extraction column in the normal-phase mode. The eluate was dried and reconstituted with acetonitrile-water (7 + 3, v/v). Chromatography was performed on a 5 microns high-carbon load C18 column with acetonitrile-water (7 + 3, v/v) at 1 mL/min and UV detection at 291 nm. Recoveries from fortified samples ranged from 84 to 116%. The limit of quantitation was 10 ppb for both beef and pork. The detection limit was 3 ppb.

  17. Liquid chromatographic analysis of oxytocin and its related substances.

    PubMed

    Ashenafi, Dunge; Van Hemelrijck, Elise; Chopra, Shruti; Hoogmartens, Jos; Adams, Erwin

    2010-01-05

    A selective gradient liquid chromatographic (LC) method for the determination of oxytocin (OT) and its related substances in bulk drugs has been developed. The method uses a reversed-phase C18 column (25 cm x 4.0 mm i.d.), 5 microm kept at 40 degrees C. The mobile phases consist of acetonitrile, dihydrogen phosphate solution pH 4.4 and water. The flow rate is 1.0 ml/min. UV detection is performed at 220 nm. A system suitability test (SST) was developed to govern the quality of the separation. The separation towards OT components was investigated on different C18 columns. The developed method was further validated with respect to robustness, precision, sensitivity and linearity. A central composite design was applied to examine the robustness of the method. The method shows good precision, sensitivity, linearity and robustness. Two commercial OT samples were examined using this method. Furthermore, the method proved to be successful when applied to analyze a marketed OT formulation for injection.

  18. Chromatographic Studies of Protein-Based Chiral Separations.

    PubMed

    Bi, Cong; Zheng, Xiwei; Azaria, Shiden; Beeram, Sandya; Li, Zhao; Hage, David S

    2016-09-01

    The development of separation methods for the analysis and resolution of chiral drugs and solutes has been an area of ongoing interest in pharmaceutical research. The use of proteins as chiral binding agents in high-performance liquid chromatography (HPLC) has been an approach that has received particular attention in such work. This report provides an overview of proteins that have been used as binding agents to create chiral stationary phases (CSPs) and in the use of chromatographic methods to study these materials and protein-based chiral separations. The supports and methods that have been employed to prepare protein-based CSPs will also be discussed and compared. Specific types of CSPs that are considered include those that employ serum transport proteins (e.g., human serum albumin, bovine serum albumin, and alpha1-acid glycoprotein), enzymes (e.g., penicillin G acylase, cellobiohydrolases, and α-chymotrypsin) or other types of proteins (e.g., ovomucoid, antibodies, and avidin or streptavidin). The properties and applications for each type of protein and CSP will also be discussed in terms of their use in chromatography and chiral separations.

  19. Gas chromatographic analysis of volatiles in fluid and gas inclusions

    USGS Publications Warehouse

    Andrawes, F.; Holzer, G.; Roedder, E.; Gibson, E.K.; Oro, J.

    1984-01-01

    Most geological samples and some synthetic materials contain fluid inclusions. These inclusions preserve for us tiny samples of the liquid and/or the gas phase that was present during formation, although in some cases they may have undergone significant changes from the original material. Studies of the current composition of the inclusions provide data on both the original composition and the change since trapping. These inclusions are seldom larger than 1 millimeter in diameter. The composition varies from a single major compound (e.g., water) in a single phase to a very complex mixture in one or more phases. The concentration of some of the compounds present may be at trace levels. We present here some analyses of inclusions in a variety of geological samples, including diamonds. We used a sample crusher and a gas chromatography-mass spectrometry (GC-MS) system to analyze for organic and inorganic volatiles present as major to trace constituents in inclusions. The crusher is a hardened stainless-steel piston cylinder apparatus with tungsten carbide crusing surfaces, and is operated in a pure helium atmosphere at a controlled temperature. Samples ranging from 1 mg to 1 g were crushed and the released volatiles were analyzed using multi-chromatographic columns and detectors, including the sensitive helium ionization detector. Identification of the GC peaks was carried out by GC-MS. This combination of procedures has been shown to provide geochemically useful information on the process involved in the history of the samples analyzed. ?? 1984.

  20. Capillary gas chromatographic analysis of pans with luminol chemilumnescent detection

    SciTech Connect

    Gaffney, J.; Bornick, R.; Chen, Yu-Harn; Marley, N.

    1996-12-31

    Peroxyacyl nitrates (PANs) are important air pollutants in tropospheric chemistry. PANs are known to be potent phytotoxins at low ppb concentrations and are lachrymators. They can also transport the more reactive nitrogen dioxide long distances, because they are in equilibrium with that NO{sub x} species. Since PANs are trapped peroxyradicals, they are a direct measure of the peroxyradical levels and the of {open_quotes}photochemical age{close_quotes} of an air parcel. The PANs are typically measured in the atmosphere by using electron capture detection methods. These methods suffer from large background signals and detector responses to oxygen and water vapor. This paper describes the combination of a capillary gas chromatographic column with a modified luminol chemiluminescent nitrogen dioxide detector (Scintrex, Luminox) for rapid and sensitive detection of nitrogen dioxide, peroxyacetyl nitrate, peroxypropionyl nitrate, and peroxybutyryl nitrate. Detection limits for this approach in the low tens of parts per trillion have been observed with total analysis times of less than three minutes. We will discuss the potential application of this method to other compounds, particularly, organonitrates, in a pyrolysis system and/or with ozone addition to the sampling streams.

  1. Biphasic Affinity Chromatographic Approach for Deep Tyrosine Phosphoproteome Analysis.

    PubMed

    Deng, Zhenzhen; Dong, Mingming; Wang, Yan; Dong, Jing; Li, Shawn S-C; Zou, Hanfa; Ye, Mingliang

    2017-02-21

    Tyrosine phosphorylation (pTyr) is important for normal physiology and implicated in many human diseases, particularly cancer. Identification of pTyr sites is critical to dissecting signaling pathways and understanding disease pathologies. However, compared with serine/threonine phosphorylation (pSer/pThr), the analysis of pTyr at the proteome level is more challenging due to its low abundance. Here, we developed a biphasic affinity chromatographic approach where Src SH2 superbinder was coupled with NeutrAvidin affinity chromatography, for tyrosine phosphoproteome analysis. With the use of competitive elution agent biotin-pYEEI, this strategy can distinguish high-affinity phosphotyrosyl peptides from low-affinity ones, while the excess competitive agent is readily removed by using NeutrAvidin agarose resin in an integrated tip system. The excellent performance of this system was demonstrated by analyzing tyrosine phosphoproteome of Jurkat cells from which 3,480 unique pTyr sites were identified. The biphasic affinity chromatography method for deep Tyr phosphoproteome analysis is rapid, sensitive, robust, and cost-effective. It is widely applicable to the global analysis of the tyrosine phosphoproteome associated with tyrosine kinase signal transduction.

  2. Comparison of three advanced chromatographic techniques for cannabis identification.

    PubMed

    Debruyne, D; Albessard, F; Bigot, M C; Moulin, M

    1994-01-01

    The development of chromatography technology, with the increasing availability of easier-to-use mass spectrometers combined with gas chromatography (GC), the use of diode-array or programmable variable-wavelength ultraviolet absorption detectors in conjunction with high-performance liquid chromatography (HPLC), and the availability of scanners capable of reading thin-layer chromatography (TLC) plates in the ultraviolet and visible regions, has made for easier, quicker and more positive identification of cannabis samples that standard analytical laboratories are occasionally required to undertake in the effort to combat drug addiction. At laboratories that do not possess the technique of GC combined with mass spectrometry, which provides an irrefutable identification, the following procedure involving HPLC or TLC techniques may be used: identification of the chromatographic peaks corresponding to each of the three main cannabis constituents-cannabidiol (CBD), delta-9-tetrahydrocannabinol (delta-9-THC) and cannabinol (CBN)-by comparison with published data in conjunction with a specific absorption spectrum for each of those constituents obtained between 200 and 300 nm. The collection of the fractions corresponding to the three major cannabinoids at the HPLC system outlet and the cross-checking of their identity in the GC process with flame ionization detection can further corroborate the identification and minimize possible errors due to interference.

  3. Novel reduced pressure-balance syringe for chromatographic analysis.

    PubMed

    Windom, Bret C; Bruno, Thomas J

    2010-11-19

    When withdrawing a fluid sample (for additional chromatographic analyses) from an apparatus operated at a reduced pressure, a typical syringe proves to be ineffective (even if it is equipped with a gas tight plunger). It simply does not create enough pressure differential to remove a fluid sample from a reduced pressure environment. We encountered such a situation as part of efforts to extend the operation of the advanced distillation curve protocol to reduced pressures. The problem was solved by the development of a pressure balance syringe that allows reliable and precise sampling from an apparatus operating at sub-ambient pressures. This new device uses an external vacuum source to evacuate a syringe barrel, allowing a user to withdraw fluid samples from environments with pressures as low as 0.5kPa. To demonstrate the operation of the newly developed device, distillate analyses were performed on two fluids at low pressure: a predefined validation mixture, and a commercial soy based biodiesel fuel. The pressure balance syringe was used successfully for sampling in both cases. The use of the pressure balance syringe is not limited to reduced pressure distillations; indeed it can be used for a variety of applications in which chemical/compositional analyses are desired on a fluid contained in a reduced pressure environment.

  4. Liquid chromatographic determination of beta-naphthoxyacetic acid in tomatoes.

    PubMed

    Gökmen, V; Acar, J

    1998-03-06

    An alternative high-performance liquid chromatographic method for the determination of beta-naphthoxyacetic acid (BNOA) in tomatoes is described. BNOA was extracted from tomatoes with acetone-dichloromethane (2:1). The extract was cleaned up by Bio-Beads S-X3 gel-permeation chromatography and by partitioning. A reversed-phase C18 column was used for HPLC analysis. The mobile phase was acetonitrile-2% acetic acid in water (50:50, v/v) pumped at a flow-rate of 1.0 ml/min. Retention time of BNOA was ca. 7 min with a percentage coefficient of variation of 0.71. Resolution of BNOA was good on the column. Percentage recoveries of BNOA were 79.5 +/- 6.82, 94.8 +/- 2.70 and 86.4 +/- 16.43 for the corresponding spiking levels of 0.5, 1.0 and 2.0 micrograms per g tomato, respectively. Analysis of 10 greenhouse tomato samples from local markets in Ankara showed no BNOA residue.

  5. Recent Advances in Water Analysis with Gas Chromatograph Mass Spectrometers

    NASA Technical Reports Server (NTRS)

    MacAskill, John A.; Tsikata, Edem

    2014-01-01

    We report on progress made in developing a water sampling system for detection and analysis of volatile organic compounds in water with a gas chromatograph mass spectrometer (GCMS). Two approaches are described herein. The first approach uses a custom water pre-concentrator for performing trap and purge of VOCs from water. The second approach uses a custom micro-volume, split-splitless injector that is compatible with air and water. These water sampling systems will enable a single GC-based instrument to analyze air and water samples for VOC content. As reduced mass, volume, and power is crucial for long-duration, manned space-exploration, these water sampling systems will demonstrate the ability of a GCMS to monitor both air and water quality of the astronaut environment, thereby reducing the amount of required instrumentation for long duration habitation. Laboratory prototypes of these water sampling systems have been constructed and tested with a quadrupole ion trap mass spectrometer as well as a thermal conductivity detector. Presented herein are details of these water sampling system with preliminary test results.

  6. Chromatographic Studies of Protein-Based Chiral Separations

    PubMed Central

    Bi, Cong; Zheng, Xiwei; Azaria, Shiden; Beeram, Sandya; Li, Zhao; Hage, David S.

    2016-01-01

    The development of separation methods for the analysis and resolution of chiral drugs and solutes has been an area of ongoing interest in pharmaceutical research. The use of proteins as chiral binding agents in high-performance liquid chromatography (HPLC) has been an approach that has received particular attention in such work. This report provides an overview of proteins that have been used as binding agents to create chiral stationary phases (CSPs) and in the use of chromatographic methods to study these materials and protein-based chiral separations. The supports and methods that have been employed to prepare protein-based CSPs will also be discussed and compared. Specific types of CSPs that are considered include those that employ serum transport proteins (e.g., human serum albumin, bovine serum albumin, and alpha1-acid glycoprotein), enzymes (e.g., penicillin G acylase, cellobiohydrolases, and α-chymotrypsin) or other types of proteins (e.g., ovomucoid, antibodies, and avidin or streptavidin). The properties and applications for each type of protein and CSP will also be discussed in terms of their use in chromatography and chiral separations. PMID:28344977

  7. Characterisation of wax works of art by gas chromatographic procedures.

    PubMed

    Regert, M; Langlois, J; Colinart, S

    2005-10-14

    To identify the various natural and synthetic substances used by sculptors at the end of the 19th century, several contemporary reference samples were investigated by high temperature gas chromatography (HT GC) and HT GC-MS. Using specific chromatographic conditions and minimising sample preparation, we could separate, detect and identify a wide range of biomolecular markers covering a great variety of molecular weights and volatilities, with a minimum amount of sample, in a single run. Beeswax, spermaceti, carnauba, candellila and Japan waxes as well as pine resin derivatives, animal fats, paraffin, ozokerite and stearin, used as additives in wax works of art, were chemically investigated. In the case of low volatile compounds, transbutylation was performed. The structure of long-chain esters of spermaceti was elucidated for the first time by HT GC-MS analysis. Such a method was then carried out on 10 samples collected on a statuette of Junon by Antoine-Louis Barye (Louvre Museum, Paris, France) and on a sculpture by Aimé-Jules Dalou (Musée de la Révolution Française, Vizille, France). The analytical results obtained provide new data on the complex recipes elaborated by sculptors at the end of the 19th century.

  8. Size exclusion chromatographic analysis of polyphenol-serum albumin complexes.

    PubMed

    Hatano, Tsutomu; Hori, Mami; Hemingway, Richard W; Yoshida, Takashi

    2003-08-01

    Formation of water-soluble polyphenol-protein complexes was investigated by size-exclusion chromatography (SEC). The combination of (-)-epigallocatechin gallate (EGCG) and bovine serum albumin (BSA), which did not form a precipitate after the solutions were mixed, showed an SEC peak due to complex formation 2-24 h after mixing. Peak size of the complex varied with time, suggesting slow change of the conformation of the protein accompanied by complexation. Formation of the complex was substantiated by ultrafiltration of the mixture; the complex did not pass through a membrane with a 100,000 nominal molecular weight limit (NMWL). The SEC profile varied with the combination of compounds. The peaks due to the complexes showed that the apparent value of the number average molecular weight (M(n)) of the EGCG-BSA complex was 2.8x10(5), while that of a pentagalloylglucose (PGG)-BSA complex was 9.5x10(5) under the conditions used. Dimeric hydrolyzable tannins, oenothein B and cornusiin A, also caused changes in the SEC profile of BSA, although the combinations did not show peaks attributable to formation of such large complexes observed for EGCG and PGG. Procyanidin B3 and (+)-catechin did not cause changes in the SEC profile of BSA. With cytochrome c, EGCG did not show any chromatographic changes.

  9. Comprehensive two-dimensional liquid chromatographic analysis of anthocyanins.

    PubMed

    Willemse, Chandré M; Stander, Maria A; Tredoux, Andreas G J; de Villiers, André

    2014-09-12

    Anthocyanins are naturally occurring plant pigments whose accurate analysis is hampered by their complexity and unique chromatographic behaviour associated with on-column conversion reactions. This paper reports the evaluation of off-line comprehensive two-dimensional liquid chromatography (LC×LC) for the analysis of anthocyanins. Hydrophilic interaction chromatography (HILIC) was used in the first dimension in combination with reversed phase liquid chromatography (RP-LC) in the second dimension. For the selective detection of anthocyanins, diode array detection was used, while high resolution quadrupole-time-of-flight mass spectrometry (Q-TOF) was used for compound identification. As application, the HILIC×RP-LC separation of diverse anthocyanins in blueberries, red radish, black beans, red grape skins and red cabbage is demonstrated. Off-line HILIC×RP-LC revealed information which could not be obtained by one-dimensional HPLC methods, while the structured elution order for the anthocyanins simplifies compound identification and facilitates the comparison of anthocyanin content of natural products by means of contour plots.

  10. Adsorption modeling for macroscopic contaminant dispersal analysis

    SciTech Connect

    Axley, J.W.

    1990-05-01

    Two families of macroscopic adsorption models are formulated, based on fundamental principles of adsorption science and technology, that may be used for macroscopic (such as whole-building) contaminant dispersal analysis. The first family of adsorption models - the Equilibrium Adsorption (EA) Models - are based upon the simple requirement of equilibrium between adsorbent and room air. The second family - the Boundary Layer Diffusion Controlled Adsorption (BLDC) Models - add to the equilibrium requirement a boundary layer model for diffusion of the adsorbate from the room air to the adsorbent surface. Two members of each of these families are explicitly discussed, one based on the linear adsorption isotherm model and the other on the Langmuir model. The linear variants of each family are applied to model the adsorption dynamics of formaldehyde in gypsum wall board and compared to measured data.

  11. Adsorption Behavior of Nonplanar Phthalocyanines: Competition of Different Adsorption Conformations

    PubMed Central

    2016-01-01

    Using density functional theory augmented with state-of-the-art van der Waals corrections, we studied the geometric and electronic properties of nonplanar chlorogallium-phthalocyanine GaClPc molecules adsorbed on Cu(111). Comparing these results with published experimental data for adsorption heights, we found indications for breaking of the metal–halogen bond when the molecule is heated during or after the deposition process. Interestingly, the work-function change induced by this dissociated geometry is the same as that computed for an intact adsorbate layer in the “Cl-down” configuration, with both agreeing well with the experimental photoemission data. This is unexpected, as the chemical natures of the adsorbates and the adsorption distances are markedly different in the two cases. The observation is explained as a consequence of Fermi-level pinning due to fractional charge transfer at the interface. Our results show that rationalizing the adsorption configurations on the basis of electronic interface properties alone can be ambiguous and that additional insight from dispersion-corrected DFT simulations is desirable. PMID:27066160

  12. Separation of chiral nanotubes with an opposite handedness by chiral oligopeptide adsorption: A molecular dynamics study.

    PubMed

    Raffaini, Giuseppina; Ganazzoli, Fabio

    2015-12-18

    The separation of enantiomeric chiral nanotubes that can form non-covalent complexes with an unlike stability upon adsorption of chiral molecules is a process of potential interest in different fields and applications. Using fully atomistic molecular dynamics simulations, we report in this paper a theoretical study of the adsorption and denaturation of an oligopeptide formed by 16 chiral amino acids having a helical structure in the native state on both the inner and the outer surface of the chiral (10, 20) and (20, 10) single-walled carbon nanotubes having an opposite handedness, and of the armchair (16, 16) nanotube with a similar diameter for comparison. In the final adsorbed state, the oligopeptide loses in all cases its native helical conformation, assuming elongated geometries that maximize its contact with the surface through all the 16 amino acids. We find that the complexes formed by the two chiral nanotubes and the chosen oligopeptide have a strongly unlike stability both when adsorption takes place on the outer convex surface of the nanotube, and when it occurs on the inner concave surface. Thus, our molecular simulations indicate that separation of chiral, enantiomeric carbon nanotubes for instance by chromatographic methods can indeed be carried out using oligopeptides of a sufficient length.

  13. Particle size effects on protein and virus-like particle adsorption on perfusion chromatography media.

    PubMed

    Wu, Yige; Abraham, Dicky; Carta, Giorgio

    2015-01-02

    The resin structure, chromatographic behavior, and adsorption kinetics of proteins and virus-like-particles (VLPs) are studied for POROS HS 20 and POROS HS 50 (23 and 52 μm mean diameter, respectively) to determine the effects of particle size on perfusion chromatography and to determine the predictive ability of available models. Transmission electron microscopy (TEM) and inverse size-exclusion chromatography (iSEC) show similar structures for the two resins, both containing 200-1000 nm pores that transect a network of much smaller pores. For non-binding conditions, trends of the height equivalent to a theoretical plate (HETP) as a function of reduced velocity are consistent with perfusion. The estimated intraparticle flow fractions for these conditions are 0.0018 and 0.00063 for POROS HS 20 and HS 50, respectively. For strong binding conditions, confocal laser scanning microscopy (CLSM) shows asymmetrical intraparticle concentrations profiles and enhanced rates of IgG adsorption on POROS HS 20 at 1000 cm/h. The corresponding effective diffusivity under flow is 2-3 times larger than for non-flow conditions and much larger than observed for POROS HS 50, consistent with available models. For VLPs, however, adsorption is confined to a thin layer near the particle surface for both resins, suggesting that the bound VLPs block the pores.

  14. Determination of organic compounds in landfill leachates treated by Fenton-Adsorption.

    PubMed

    Ramírez-Sosa, Dorian R; Castillo-Borges, Elba R; Méndez-Novelo, Roger I; Sauri-Riancho, María R; Barceló-Quintal, Manuel; Marrufo-Gómez, José M

    2013-02-01

    The objective of this study was to identify the organic compounds removed from the leachate when treated with Fenton-Adsorption by gas chromatography coupled to mass spectrometry (GC-MS) in order to identify toxic compounds that could be harmful for the environment or human health. The physicochemical characterization of the raw leachate was carried out before and after the Fenton-Adsorption process. The effluent from each stage of this process was characterized: pH, Biological Oxygen Demand (BOD(5)), Chemical Oxygen Demand (COD), Total Organic Carbon (TOC), Total Carbon (TC), Inorganic Carbon (IC), Total Solids (TS), Total Suspended Solids (TSS) and Color. The organic compounds were determined by GC-MS. The removal of COD and color reached over 99% in compliance with the Mexican Standard NOM-001-SEMARNAT-1996, which establishes the maximum permissible limits for contaminants present in wastewater discharges to water and national goods. The chromatographic analysis from the Fenton-Adsorption effluent proved that this treatment removed more than 98% of the organic compounds present in the initial sample. The mono (2-ethylhexyl) ester 1,2-benzenedicarboxylic acid persisted, although it is not considered as toxic compound by the NOM-052-SEMARNAT-2005. Therefore, the treated effluent can be safely disposed of into the environment.

  15. Consequences of cavity size and chemical environment on the adsorption properties of isoreticular metal-organic frameworks: an inverse gas chromatography study.

    PubMed

    Gutiérrez, Inés; Díaz, Eva; Vega, Aurelio; Ordóñez, Salvador

    2013-01-25

    The role of the structure of three isoreticular metal-organic frameworks (IRMOFs) on their adsorption behavior has been studied in this work, selecting different kinds of volatile organic compounds (VOCs) as adsorbates (alkanes, alkenes, cycloalkanes, aromatics and chlorinated). For this purpose, three samples (IRMOF-1, IRMOF-8 and IRMOF-10) with cubic structure and without functionalities on the organic linkers were synthesized. Adsorption capacities at infinite dilution were derived from the adsorption isotherms, whereas thermodynamic properties have been determined from chromatographic retention volume. The capacity and the strength of adsorption were strongly influenced by the adsorbate size. This effect is especially relevant for n-alkanes adsorption, indicating the key role of the cavity size on this phenomenon, and hence the importance of the IRMOF structural properties. A different behavior has been observed for the polar compounds, where an enhancement on the specificity of the adsorption with the π-electron rich regions was observed. This fact suggests the specific interaction of these molecules with the organic linkers of the IRMOFs.

  16. Reversed-phase liquid chromatographic determination of cromolyn sodium in drug substance and select dosage forms.

    PubMed

    Ng, L L

    1994-01-01

    This study, presented as a technical communication, describes a reversed-phase liquid chromatographic method for select commercial formulations, namely, inhalation solution, nasal solution, capsule and inhalation aerosol. Miscellaneous validation parameters are also discussed.

  17. DEVELOPMENT AND VALIDATION OF AN ION CHROMATOGRAPHIC METHOD FOR DETERMINING PERCHLORATE IN FERTILIZERS

    EPA Science Inventory

    A method has been developed for the determination of perchlorate in fertilizers. Materials are leached with deionized water to dissolve any soluble perchlorate compounds. Ion chromatographic separation is followed by suppressed conductivity for detection. Perchlorate is retained ...

  18. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  19. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  20. 21 CFR 862.2230 - Chromatographic separation material for clinical use.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... chromatographic separation material for clinical use is a device accessory (e.g., ion exchange absorbents, ion exchagne resins, and ion papers) intended for use in ion exchange chromatography, a procedure in which...

  1. Oxygen carrier for gas chromatographic analysis of inert gases in propellants

    NASA Technical Reports Server (NTRS)

    Cannon, W. A.

    1972-01-01

    Gas chromatographic determination of small quantities of inert gases in reactive propellants is discussed. Operating conditions used for specific analyses of helium in diborane and nitrogen in oxygen difluoride are presented in tabular form.

  2. A Miniature Gas Chromatograph Mass Spectrometer (GCMS) for Planetary Atmospheres Studies

    NASA Astrophysics Data System (ADS)

    Simcic, J.; Madzunkov, S. M.; Bae, B.; Nikolic, D.; Darrach, M.

    2016-10-01

    Presented herein are the latest achievements in developing an instrument with the same analytical performance of commercial Gas Chromatograph Mass Spectrometer systems but approximately an order of magnitude smaller and optimized for space missions.

  3. HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

    EPA Science Inventory

    High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) was obtained on polysaccharide enantioselective HPLC columns using alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, fonofos, fenamiph...

  4. Studies on Vapor Adsorption Systems

    NASA Technical Reports Server (NTRS)

    Shamsundar, N.; Ramotowski, M.

    1998-01-01

    The project consisted of performing experiments on single and dual bed vapor adsorption systems, thermodynamic cycle optimization, and thermal modeling. The work was described in a technical paper that appeared in conference proceedings and a Master's thesis, which were previously submitted to NASA. The present report describes some additional thermal modeling work done subsequently, and includes listings of computer codes developed during the project. Recommendations for future work are provided.

  5. Chromatographic extraction with di(2-ethylhexyl)orthophosphoric acid for production and purification of promethium-147

    DOEpatents

    Boll, Rose A [Knoxville, TN

    2008-10-14

    A method of producing and purifying promethium-147 including the steps of: irradiating a target material including neodymium-146 with neutrons to produce promethium-147 within the irradiated target material; dissolving the irradiated target material to form an acidic solution; loading the acidic solution onto a chromatographic separation apparatus containing HDEHP; and eluting the apparatus to chromatographically separate the promethium-147 from the neodymium-146.

  6. High-resolution gas chromatographic profiles of volatile organic compounds produced by microorganisms at refrigerated temperatures.

    PubMed Central

    Lee, M L; Smith, D L; Freeman, L R

    1979-01-01

    Three different strains of bacteria isolated from spoiled, uncooked chicken were grown in pure culture on Trypticase soy agar supplemented with yeast extract. The volatile organic compounds produced by each culture were concentrated on a porous polymer precolumn and analyzed by high-resolution gas chromatographic mass spectrometry. Twenty different compounds were identified. Both qualitative and quantitative differences in the chromatographic profiles from each culture were found. PMID:104660

  7. Multidimensional High-Resolution Gas Chromatographic Investigations of Hydrocarbon Fuels and Various Turbine Engine Fuel Precursors.

    DTIC Science & Technology

    1985-08-01

    Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy . 15. B. Welton, Column Switching and Backflush Techniques with Open Tubular and...Packed Columns in Gas Chromatography, Paper presented at 1978 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy . 16. R. Miller... Applied Spectroscopy . 33. J. F. Pankow and L. M. Isabelle, Interface of the Direct Coupling of a Second Gas Chromatograph to a Gas Chromatograph/ Mass

  8. Hydrogen Adsorption in Carbon nanoparticles

    NASA Astrophysics Data System (ADS)

    Cabrera, A. L.; Rojas, S.; Dias-Droguett, D. E.; Bhuyan, H.; Aomoa, N.; Kakati, M.

    2013-03-01

    We have studied hydrogen adsorption in carbon nanoparticles using a quartz crystal microbalance. The carbon nanoparticles were synthesized from a thermal plasma jet at different pressure (15 - 263 torr) of the reactants and different current (50 - 250 A) to generate the plasma. The as-prepared carbon nanoparticles were directly deposited on top of the gold electrode of a quartz crystal and we monitored in-situ the changes in resonance frequency while the chamber was pressurized at different hydrogen pressures. These changes enabled determination of absorbed hydrogen mass in order to get H/C mass ratio curves as a function of H2 pressure. Adsorption curves obtained in some carbon nanoparticles indicated the formation of hydrogen monolayer inside the pores of the carbon nanoparticles. Using the value of the jump due to the formation of a H2\\ monolayer, a surface area was estimated between 40-60 m2/g for hydrogen adsorption. In other carbon samples, hydrogen uptake curves indicated that H2 was filling the sample's pores when pore volume was large. These observations will be discussed in detail for several carbon nanoparticles samples. Funds provided by VRI Puente 9/2012 and 10/2012

  9. Adsorption of Gemini surfactants onto clathrate hydrates.

    PubMed

    Salako, O; Lo, C; Couzis, A; Somasundaran, P; Lee, J W

    2013-12-15

    This work addresses the adsorption of two Gemini surfactants at the cyclopentane (CP) hydrate-water interface. The Gemini surfactants investigated here are Dowfax C6L and Dowfax 2A1 that have two anionic head groups and one hydrophobic tail group. The adsorption of these surfactants was quantified using adsorption isotherms and the adsorption isotherms were determined using liquid-liquid titrations. Even if the Gemini surfactant adsorption isotherms show multi-layer adsorption, they possess the first Langmuir layer with the second adsorption layer only evident in the 2A1 adsorption isotherm. Zeta potentials of CP hydrate particles in the surfactant solution of various concentrations of Dowfax C6L and Dowfax 2A1 were measured to further explain their adsorption behavior at the CP hydrate-water interface. Zeta potentials of alumina particles as a model particle system in different concentrations of sodium dodecyl sulfate (SDS), Dowfax C6L and Dowfax 2A1 were also measured to confirm the configuration of all the surfactants at the interface. The determination of the isotherms and zeta-potentials provides an understanding framework for the adsorption behavior of the two Gemini surfactants at the hydrate-water interface.

  10. Liquid chromatographic analysis of cinchona alkaloids in beverages.

    PubMed

    Horie, Masao; Oishi, Mitsuo; Ishikawa, Fusako; Shindo, Tetsuya; Yasui, Akiko; Ogino, Shuzo; Ito, Koichi

    2006-01-01

    A method for the determination of Cinchona extract (whose main components are the alkaloids cinchonine, cinchonidine, quinidine, and quinine) in beverages by liquid chromatography was developed. A beverage with an alcohol content of more than 10% was loaded onto an OASIS HLB solid-phase extraction cartridge, after it was adjusted to pH 10 with 28% ammonium hydroxide. Other beverages were centrifuged at 4000 rpm for 5 min, and the supernatant was loaded onto the cartridge. The cartridge was washed with water followed by 15% methanol, and the Cinchona alkaloids were eluted with methanol. The Cinchona alkaloids in the eluate were chromatographed on an L-column ODS (4.6 mm id x 150 mm) with methanol and 20 mmol/L potassium dihydrogen phosphate (3 + 7) as the mobile phase. Cinchona alkaloids were monitored with an ultraviolet (UV) detector at 230 nm, and with a fluorescence detector at 405 nm for cinchonine and cinchonidine and 450 nm for quinidine and quinine (excitation at 235 nm). The calibration curves for Cinchona alkaloids with the UV detector showed good linearity in the range of 2-400 microg/mL. The detection limit of each Cinchona alkaloid, taken to be the concentration at which the absorption spectrum could be identified, was 2 microg/mL. The recovery of Cinchona alkaloids added at a level of 100 microg/g to various kinds of beverages was 87.6-96.5%, and the coefficients of variation were less than 3.3%. A number of beverage samples, some labeled to contain bitter substances, were analyzed by the proposed method. Quinine was detected in 2 samples of carbonated beverage.

  11. Ion chromatographic identification and quantification of glycol degradation products.

    PubMed

    Madera, M; Höflinger, W; Kadnar, R

    2003-05-16

    In water-based heat transfer systems, frequently glycols are added to the water to obtain freeze protection. For this purpose, ethylene glycol (EG) is the most common substance used. When heated, the glycol will slowly degrade and the pH of the glycol-water mixture will decrease, leading to corrosion and foaming problems. Carboxylic acids were identified as the main degradation products. Quantification of the carboxylic acids is of importance to monitor the degradation reactions in order to identify hot spots or overheating, caused by severe heat exchanger scaling, where pH measurements will not be sufficient due to buffer substances added for corrosion protection. In this work, ion chromatographic methods havebeen developed to identify the main degradation products of EG in heat transfer systems and to monitor the degradation process. Possible acidic reaction products of EG are glycolic acid, glyoxylic acid, oxalic acid, acetic acid and formic acid. Separations with a Dionex AS9-HC column with Na2CO3 eluents of differing concentrations showed that only trace amounts of carboxylic acids are present in aged heat transfer media. Oxalic acid can be quantified simultaneously to nitrite or molybdate which are added as corrosion inhibitors. A Dionex AS10 separation column with Na2B4O7 eluent enabled base line separation of glycolic acid, acetic acid and formic acid. Heat transfer media, which are operated in different heat transfer systems under different conditions, were analysed. A system was identified, where severe overheating due to fluid maldistribution in the heat exchanger took place.

  12. Liquid chromatographic determination of seven antioxidants in dry food.

    PubMed

    Page, B D; Charbonneau, C F

    1989-01-01

    The liquid chromatographic determinative step of the official method for propyl gallate, trihydroxybutyrophenone, tert-butylhydroquinone, nordihydroguaiaretic acid, butylated hydroxyanisole (BHA), 3,5-di-tert-butyl-4-hydroxymethylphenol, and butylated hydroxytoluene (BHT) in fats and oils has been applied to their determination in a number of dry foods. A representative sample (10 g) is homogenized first with hexane (25 mL), then with 5 mL added water, and finally with 75 mL added acetonitrile. The hexane and acetonitrile are decanted, filtered, and separated; the hexane and rehydrated food are reextracted with 2 additional portions of acetonitrile, and the combined acetonitrile extracts are concentrated and diluted to 10 mL. An aliquot is analyzed as described in the official method, using a 150 x 4.6 mm 5 microns C-18 column. The need for rehydration to maximize the recovery of BHA and other antioxidants from marketplace dry food samples such as potato flakes, dry coffee whiteners, and dessert topping mixes was demonstrated. Rehydration was not required for cheese snacks, breakfast cereals, cake mixes, and some other foods. The need for rehydration should be determined by analyzing other foods with and without the addition of water. Potato and corn chips, popcorn and cheese snacks, breakfast cereals, dry beverage mixes, rice, potato flakes, french fried potatoes, and cake mixes were spiked with the above antioxidants at 10-50 ppm. Overall recoveries ranged from 64.3 to 105.6% and repeatabilities ranged from 0.7 to 10.8%. A total of 109 samples of the above foods were analyzed, and 64% contained detectable (greater than 1-2 ppm) antioxidants, mainly BHA and BHT.

  13. Gas chromatographic determination of yohimbine in commercial yohimbe products.

    PubMed

    Betz, J M; White, K D; der Marderosian, A H

    1995-01-01

    The bark of Pausinystalia yohimbe [K. Schumann] Pierre (Rubiaceae), long valued as an aphrodisiac in West Africa, recently has been promoted in the United States as a dietary supplement alternative to anabolic steroids for enhancement of athletic performance. As the number of yohimbe products on the retail market increases, concerns about their safety are raised because of the reported toxicity of yohimbine (the major alkaloid of the plant). Although plant materials are usually identified microscopically, we were unable to identify them in many of the products, because as their labels indicated, the products were mixtures of various botanicals or were bark extracts and contained little or no plant material. A method for extraction and capillary gas chromatographic (GC) separation of the alkaloids of P. yohimbe was, therefore, developed and used to analyze a number of commercial yohimbe products. The method involved solvent extraction and partitioning in chloroform-water followed by separation on a methyl silicone capillary GC column (N-P detection). Comparisons of chromatograms of extracts of authentic bark with those of commercial products indicated that, although many products contained measurable quantities of the alkaloid yohimbine, they were largely devoid of the other alkaloids previously reported in this species. Concentrations of yohimbine in the commercial products ranged from < 0.1 to 489 ppm, compared with 7089 ppm in the authentic material. Authentic bark has been reported to contain up to 6% total alkaloids, 10-15% of which are yohimbine. The possible presence of undeclared diluents in the products was indicated by peaks in product chromatograms but not in those of authentic bark.

  14. Chromatographic fingerprint similarity analysis for pollutant source identification.

    PubMed

    Xie, Juan-Ping; Ni, Hong-Gang

    2015-12-01

    In the present study, a similarity analysis method was proposed to evaluate the source-sink relationships among environmental media for polybrominated diphenyl ethers (PBDEs), which were taken as the representative contaminants. Chromatographic fingerprint analysis has been widely used in the fields of natural products chemistry and forensic chemistry, but its application to environmental science has been limited. We established a library of various sources of media containing contaminants (e.g., plastics), recognizing that the establishment of a more comprehensive library allows for a better understanding of the sources of contamination. We then compared an environmental complex mixture (e.g., sediment, soil) with the profiles in the library. These comparisons could be used as the first step in source tracking. The cosine similarities between plastic and soil or sediment ranged from 0.53 to 0.68, suggesting that plastic in electronic waste is an important source of PBDEs in the environment, but it is not the only source. A similarity analysis between soil and sediment indicated that they have a source-sink relationship. Generally, the similarity analysis method can encompass more relevant information of complex mixtures in the environment than a profile-based approach that only focuses on target pollutants. There is an inherent advantage to creating a data matrix containing all peaks and their relative levels after matching the peaks based on retention times and peak areas. This data matrix can be used for source identification via a similarity analysis without quantitative or qualitative analysis of all chemicals in a sample.

  15. High ionic strength narrows the population of sites participating in protein ion-exchange adsorption: a single-molecule study.

    PubMed

    Kisley, Lydia; Chen, Jixin; Mansur, Andrea P; Dominguez-Medina, Sergio; Kulla, Eliona; Kang, Marci K; Shuang, Bo; Kourentzi, Katerina; Poongavanam, Mohan-Vivekanandan; Dhamane, Sagar; Willson, Richard C; Landes, Christy F

    2014-05-23

    The retention and elution of proteins in ion-exchange chromatography is routinely controlled by adjusting the mobile phase salt concentration. It has repeatedly been observed, as judged from adsorption isotherms, that the apparent heterogeneity of adsorption is lower at more-eluting, higher ionic strength. Here, we present an investigation into the mechanism of this phenomenon using a single-molecule, super-resolution imaging technique called motion-blur Points Accumulation for Imaging in Nanoscale Topography (mbPAINT). We observed that the number of functional adsorption sites was smaller at high ionic strength and that these sites had reduced desorption kinetic heterogeneity, and thus narrower predicted elution profiles, for the anion-exchange adsorption of α-lactalbumin on an agarose-supported, clustered-charge ligand stationary phase. Explanations for the narrowing of the functional population such as inter-protein interactions and protein or support structural changes were investigated through kinetic analysis, circular dichroism spectroscopy, and microscopy of agarose microbeads, respectively. The results suggest the reduction of heterogeneity is due to both electrostatic screening between the protein and ligand and tuning the steric availability within the agarose support. Overall, we have shown that single molecule spectroscopy can aid in understanding the influence of ionic strength on the population of functional adsorbent sites participating in the ion-exchange chromatographic separation of proteins.

  16. High ionic strength narrows the population of sites participating in protein ion-exchange adsorption: A single-molecule study

    PubMed Central

    Kisley, Lydia; Chen, Jixin; Mansur, Andrea P.; Dominguez-Medina, Sergio; Kulla, Eliona; Kang, Marci; Shuang, Bo; Kourentzi, Katerina; Poongavanam, Mohan-Vivekanandan; Dhamane, Sagar; Willson, Richard C.; Landes, Christy F.

    2014-01-01

    The retention and elution of proteins in ion-exchange chromatography is routinely controlled by adjusting the mobile phase salt concentration. It has repeatedly been observed, as judged from adsorption isotherms, that the apparent heterogeneity of adsorption is lower at more-eluting, higher ionic strength. Here, we present an investigation into the mechanism of this phenomenon using a single-molecule, super-resolution imaging technique called motion-blur Points Accumulation for Imaging in Nanoscale Topography (mbPAINT). We observed that the number of functional adsorption sites was smaller at high ionic strength and that these sites had reduced desorption kinetic heterogeneity, and thus narrower predicted elution profiles, for the anion-exchange adsorption of α-lactalbumin on an agarose-supported, clustered-charge ligand stationary phase. Explanations for the narrowing of the functional population such as inter-protein interactions and protein or support structural changes were investigated through kinetic analysis, circular dichroism spectroscopy, and microscopy of agarose microbeads, respectively. The results suggest the reduction of heterogeneity is due to both electrostatic screening between the protein and ligand and tuning the steric availability within the agarose support. Overall, we have shown that single molecule spectroscopy can aid in understanding the influence of ionic strength on the population of functional adsorbent sites participating in the ion-exchange chromatographic separation of proteins. PMID:24751557

  17. Combined HPLC/HPSEC study of Suwannee River Fulvic Acid adsorptive fractionation on α-aluminum oxide.

    PubMed

    Kreller, David I; Schlautman, Mark A; McGunigale, Samantha L

    2013-01-15

    A novel liquid chromatographic (LC) method with repeated injections of Suwannee River Fulvic Acid (SRFA) was used to investigate its adsorptive fractionation by synthetic α-Al(2)O(3). Eluent (i.e., non-retained) SRFA for each injection was monitored by two ultraviolet (UV) absorbance detection channels (300 and 365 nm) and one fluorescence detection channel (λ(ex)=350 nm, λ(em)=450 nm). Preferential adsorption of SRFA constituents was revealed by the different responses of the three LC detection channels. Samples of non-retained SRFA from injections of three independent replicate experiments were collected and aggregated for subsequent analysis by steady state ultraviolet-visible (UV/vis) absorption spectrometry and size exclusion chromatography (SEC). The ratio of absorbance at 254 and 204 nm, a surrogate for specific UV absorbance at 254 nm, increased with increasing injection number for the non-retained SRFA, indicating the preferential adsorption of SRFA constituents containing aromatic moieties. SEC analysis confirmed the preferential adsorption of higher molecular weight (MW) SRFA constituents as the non-adsorbed SRFA fractions increased in MW across the series of injections. The SEC results also suggested that certain SRFA constituents in the ca. 2-5 kDa MW range adsorbed in early injections were displaced by higher MW species (ca. 5-10 kDa) in later injections.

  18. DNA stickers promote polymer adsorption onto cellulose.

    PubMed

    Sato, Teruaki; Ali, Md Monsur; Pelton, Robert; Cranston, Emily D

    2012-10-08

    Adsorption of oligonucleotides onto model cellulose surfaces was investigated by comparing the Boese and Breaker's cellulose binding oligonucleotide (CBO) with a nonspecific oligonucleotide control (NSO). Measurements using the quartz crystal microbalance with dissipation technique confirmed that CBO adsorbed onto cellulose more than NSO, particularly at high ionic strengths (100 mM CaCl(2)). CBO showed a higher maximum adsorption on nanofibrillated and nanocrystalline cellulose than on regenerated cellulose, indicating a preference for the native cellulose I crystal structure under conditions that favored specific adsorption over calcium-mediated electrostatically driven adsorption. In addition, an anionic polyacrylamide (A-PAM) with grafted CBO also adsorbed onto the surface of cellulose in CaCl(2), whereas the unmodified A-PAM did not. This work shows that CBO performs as a "sticker", facilitating the adsorption of polyacrylamide onto cellulose, even under high ionic strength conditions where the adsorption of conventional polyelectrolytes is inhibited.

  19. Adsorption of goethite onto quartz and kaolinite

    USGS Publications Warehouse

    Goldberg, M.C.; Weiner, Eugene R.; Boymel, P.M.

    1984-01-01

    The adsorption of colloidal goethite onto quartz and kaolinite substrates has been studied as a function of pH and NaCl concentration. Goethite adsorption was measured quantitatively by Fourier-transform infrared spectroscopy. The results indicate that adsorption onto both substrates is due primarily to coulombic forces; however, the pH dependence of adsorption is very different for the two substrates. This is explained by the fact that the surface charge on quartz is entirely pH-dependent, while kaolinite has surface faces which carry a permanent negative charge. Adsorption of goethite on to kaolinite increases markedly with increasing NaCl concentration, while adsorption onto quartz is relatively independent of NaCl concentration. This can be explained by the influence of NaCl concentration upon the development of surface charge on the substrates. A method is described for separating surface-bound goethite from free goethite.

  20. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column.

    PubMed

    Arai, Kaori; Mori, Masanobu; Hironaga, Takahiro; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2012-04-01

    A combination of hydrophilic interaction chromatographic (HILIC) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography (IC). Firstly, the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions. The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10). When using tartaric acid as the eluent, the HILIC columns indicated strong retentions for anions, based on ion-pair interaction. Especially, HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I(-) > NO3(-) > Br(-) > Cl(-) > H2PO4(-). However, since HILIC-10 could not separate analyte cations, a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series. The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+, NH4+, K+, Mg2+, Ca2+, H2PO4(-), Cl(-), Br(-), NO3(-) and I(-)) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6. The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections. The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 micromol/L for the cations and 0.31 - 1.2 micromol/L for the anions. This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

  1. The role of surface heterogeneity and lateral interactions in the adsorption of volatile organic compounds on rutile surface

    NASA Astrophysics Data System (ADS)

    Metaxa, E.; Kolliopoulos, A.; Agelakopoulou, T.; Roubani-Kalantzopoulou, F.

    2009-04-01

    Volatile organic compounds (VOCs) are pollutants of great interest because they are very harmful for both human health and the environment, even at very low concentrations. In this work we present and discuss the results of the experimental chromatographic study of the role of surface heterogeneity and lateral interactions in the adsorption of volatile organic compounds - ethanol, acetaldehyde and acetone - on the surface of rutile (TiO 2), a typical oxide widely used as a white pigment and a photocatalyst, as well. The ethanol, acetaldehyde and acetone were chosen because they contain the same heteroatom (O) and they have small carbon-chains. The novel method of Reversed Flow-Inverse Gas Chromatography is used, which has a powerful mathematical background and comprises a simple experimental arrangement for the determination of energetic physicochemical quantities directly from the experimental data, by means of a time-resolved analysis. In particular, several important physicochemical quantities are determined, as local adsorption energy, local adsorption isotherm, local monolayer capacity, non-adsorbed gaseous concentration of adsorbate, density probability function for the adsorption energy values, as well as the differential energy of adsorption due to lateral interactions among molecules adsorbed on the heterogeneous solid surface of TiO 2. By means of these quantities, appropriate answers are achieved to critical questions of: (a) What is the type of the adsorption isotherm of a system? (b) Where are the adsorbed molecules located on the heterogeneous surface? (c) What is the nature of the surface bonds? (d) What is the type of non-ideality of the system and (e) How does the adsorbate affect the adsorbent properties?

  2. Adsorption and isotopic fractionation of Xe

    NASA Technical Reports Server (NTRS)

    Bernatowicz, T. J.; Podosek, F. A.

    1986-01-01

    A theoretical description of the mechanisms of isotopic fractionation arising during adsorption of noble gases in a Henry's Law pressure regime is given. Experimental data on the isotopic composition of Xe adsorbed on activated charcoal in the temperature range 220 K to 350 K are presented. Both theoretical considerations and the experimental data indicate that equilibrium adsorption does not significantly alter the isotopic structure of adsorbed structure of adsorbed noble gases. Therefore, if adsorption is responsible for the elemental noble gas pattern in meteorites and the earth, the heavy noble gas isotopic fractionation between them must have been produced prior to and by a different process than equilibrium adsorption.

  3. Adsorption of water vapor on reservoir rocks

    SciTech Connect

    Not Available

    1993-07-01

    Progress is reported on: adsorption of water vapor on reservoir rocks; theoretical investigation of adsorption; estimation of adsorption parameters from transient experiments; transient adsorption experiment -- salinity and noncondensible gas effects; the physics of injection of water into, transport and storage of fluids within, and production of vapor from geothermal reservoirs; injection optimization at the Geysers Geothermal Field; a model to test multiwell data interpretation for heterogeneous reservoirs; earth tide effects on downhole pressure measurements; and a finite-difference model for free surface gravity drainage well test analysis.

  4. Adsorption of acid dye onto organobentonite.

    PubMed

    Baskaralingam, P; Pulikesi, M; Elango, D; Ramamurthi, V; Sivanesan, S

    2006-02-06

    Removal of Acid Red 151 from aqueous solution at different dye concentrations, adsorbent doses and pH has been studied. The bentonite clay has been modified using cationic surfactants, which has been confirmed using XRD and FT-IR analyses. Experimental result has shown that the acidic pH favours the adsorption. The adsorption isotherms are described by means of Langmuir and Freundlich isotherms. The adsorption capacity has been found to be 357.14 and 416.66 mg g(-1) for the cetyldimethylbenzylammonium chloride-bentonite (CDBA-bent) and cetylpyridinium chloride-bentonite (CP-bent), respectively. Kinetic studies show that the adsorption followed second-order kinetics.

  5. Ozone adsorption on carbon nanoparticles

    NASA Astrophysics Data System (ADS)

    Chassard, Guillaume; Gosselin, Sylvie; Visez, Nicolas; Petitprez, Denis

    2014-05-01

    Carbonaceous particles produced by incomplete combustion or thermal decomposition of hydrocarbons are ubiquitous in the atmosphere. On these particles are adsorbed hundreds of chemical species. Those of great concern to health are polycyclic aromatic hydrocarbons (PAHs). During atmospheric transport, particulate PAHs react with gaseous oxidants. The induced chemical transformations may change toxicity and hygroscopicity of these potentially inhalable particles. The interaction between ozone and carbon particles has been extensively investigated in literature. However ozone adsorption and surface reaction mechanisms are still ambiguous. Some studies described a fast catalytic decomposition of ozone initiated by an atomic oxygen chemisorption followed by a molecular oxygen release [1-3]. Others suggested a reversible ozone adsorption according to Langmuir-type behaviour [4,5]. The aim of this present study is a better understanding of ozone interaction with carbon surfaces. An aerosol of carbon nanoparticles was generated by flowing synthetic air in a glass tube containing pure carbon (primary particles < 50 nm), under magnetic stirring. The aerosol was then mixed with ozone in an aerosol flow tube. Ozone uptake experiments were performed with different particles concentrations with a fixed ozone concentration. The influence of several factors on kinetics was examined: initial ozone concentration, particle size (50 nm ≤ Dp ≤ 200 nm) and competitive adsorption (with probe molecule and water). The effect of initial ozone concentration was first studied. Accordingly to literature, it has been observed that the number of gas-phase ozone molecules lost per unit particle surface area tends towards a plateau for high ozone concentration suggesting a reversible ozone adsorption according to a Langmuir mechanism. We calculated the initial reaction probability between O3 and carbon particles.An initial uptake coefficient of 1.10-4 was obtained. Similar experiments were

  6. Comparison of physicochemical and gas chromatographic polarity measures for simple organic compounds.

    PubMed

    Héberger, Károly; Zenkevich, Igor G

    2010-04-23

    The comparison of different polarity measures (parameters, descriptors, variables, scales, etc.) indicates that evaluation of interrelations between these measures is important for better understanding and interpretation of chemical and/or analytical data, especially for chromatographic separation. The best linear correlation between gas chromatographic and non-chromatographic polarity descriptors is revealed for the first time: this pair of variables is the difference of gas chromatographic retention indices on standard polar and non-polar phases as well as the difference between non-dimensional indices of boiling points (known in chromatography since mid-1980s as dispersion indices) and indices of molar refractions. The correlation helps chromatographers to find preferable chemical variables (features) to understand better the separation phenomena and to find better correlations in QSRR models. Principal component analysis (PCA) of ten frequently applied polarity measures shows their similarity and, at the same time, it shows the absence of anomalies within the set of simple organic molecules. A novel ranking method for ten polarity parameters points out that the two most informative polarity measures are (i) the non-dimensional index for boiling point and (ii) the difference in chromatographic retention indices on standard polar and non-polar stationary phases. On the other hand, the hydrophobicity parameter, log P, sometimes considered as polarity parameter in HPLC seems to be the worst one in description of "polarity" in gas chromatography. Surprisingly, such polarity measures like dipole moment and permittivity used often in organic chemistry does not provide the best correlation with gas chromatographic polarity measures.

  7. Liquid chromatographic methods for biotransformation studies of ochratoxin A.

    PubMed

    Schaut, A; De Saeger, S; Sergent, T; Schneider, Y-J; Larondelle, Y; Pussemier, L; Blank, R; Van Peteghem, C

    2008-09-01

    Liquid chromatographic methods were used for the detection of ochratoxin A (OTA) and its metabolites ochratoxin alpha (OTalpha), 10-hydroxy OTA (10-OHOTA), 4R-hydroxy OTA (4R-OHOTA) and the ethyl ester of OTA (OTC) in in vitro samples, obtained with Caco-2 cell culture experiments and in in vivo urine samples from sheep. A high-performance liquid chromatography method with fluorescence detection (HPLC-FLD) and a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method were developed and validated for the detection of OTA and its metabolites OTalpha, 10-OHOTA, 4R-OHOTA and OTC, which was used as internal standard. The LOD/LOQ values for OTalpha, 4R-OHOTA and OTA were 0.63/2.11, 0.99/3.31 and 0.84/2.81 microg/L, respectively, for the HPLC-FLD method and 0.98/3.28, 1.11/3.72 and 0.88/2.96 microg/L, respectively for the LC-MS/MS method. Within-day and between-day precision were both <12% for the HPLC-FLD method, and <10% for the LC-MS/MS method. The recovery of OTA and its metabolites ranged between 71 and 111% for the HPLC-FLD method and between 79 and 110% for the LC-MS/MS method. In the first experiment only OTA was added to the Caco-2 cells while in the second experiment 3-methylcholanthrene (3MC) was also present in the cell culture systems. Besides OTA, which was recovered in all the samples, an unknown compound was also observed in the second experiment. When 3MC was added, the results showed that the OTA concentration in the basolateral samples was decreased by 50%. The methods were also implemented for the analysis of urine samples of sheep, fed increasing amounts of OTA. With the HPLC-FLD method it could be concluded that the concentration of OTA and OTalpha increased according to ingested amounts of OTA, with OTalpha being the most abundant compound. The results obtained with the LC-MS/MS method confirmed these results.

  8. Liquid chromatographic separation of antidepressant drugs: I. Tricyclics.

    PubMed

    Beierle, F A; Hubbard, R W

    1983-01-01

    A simple normal-phase (silica), high-performance liquid chromatographic (HPLC) assay of amitriptyline (AMI), doxepin (DOX), imipramine (IMI), nortriptyline (NORT), desmethyldoxepin (DESDOX), desipramine (DESIP), and protriptyline (PRO) in serum with no coelution is described here. Trimipramine and promazine were used as internal standards. Extraction of the 1.0-ml serum samples (collected in plastic) was done with Bond-Elut C18 columns. The compounds of interest were eluted with 10 mM methanolic ammonium acetate. The eluates were evaporated at 56-58 degrees C and reconstituted with 200 microliters of the mobile phase. The mobile phase was absolute ethanol-acetonitrile-tert-butylamine (98:2:0.05, vol/vol/vol). Detection of eluted drugs was at 254 nm at 0.01 absorbance units full scale (AUFS), except for PRO, which was detected at 229 nm at 0.02 AUFS. Absolute recoveries were 87-97%. A 5-micron silica (4.6 X 250 mm) HPLC column was used; results with a 10-micron silica column (3.9 X 300 mm) are also presented. Peak height ratios with trimipramine were linear for each analyte between 25 and 1200 ng/ml. Peak height ratios with promazine as the internal standard were linear for each analyte between 25 and 600 ng/ml. Detection limits under the conditions described were 2 ng/ml for AMI, DOX, and IMI, 4 ng/ml for NORT, DESDOX, and DESIP, and 10 ng/ml for PRO. Coefficients of within-day and day-to-day variation at three concentration levels were less than 9.8% and less than 11.2%, respectively. The hydroxylated metabolites of IMI, DES, NORT, and the cis isomer of DOX are discussed. Steady-state daily dosages and corresponding serum levels are presented for 69 patients. The total assay time was less than 10 min for DESIP and 12 min for PRO. This assay can be used in correlating serum levels with clinical effects, compliancy, and pharmacokinetic studies.

  9. Anion adsorption induced surface reconstructions

    NASA Astrophysics Data System (ADS)

    Tang, Lei

    2005-11-01

    Surface stress plays an important role in the behavior of solid surfaces. Potential-controlled anion adsorption in electrolytes alters the surface stress of the electrode and results in morphology changes to the surfaces. With a combination of potential-induced surface stress measurement and in situ electrochemical scanning tunneling microscopy (STM), it is demonstrated that anion adsorption induces changes in structure of thin films and modifies the growth morphology and stress evolution in epitaxially grown films. Surface structural transitions in the heteroepitaxial system consisting of one to two gold monolayers on platinum substrates were observed. By increasing the potential, structural transitions, from (1 x 1), to a striped phase, to a hexagonal structure, occurred in the gold bilayer. This hexagonal structure was related to the formation of an ordered sulfate adlayer with a ( 3x7 ) structure. Such transitions were repeatable by cycling the potential. Furthermore, the transitions between various dislocation structures were affected by anion adsorption. The surface composition of the gold bilayer on Pt was measured by underpotential deposition of copper. By subtracting the contribution of a pure Pt surface from the gold bi-layer on Pt, a stress change of -2.4 N/m was observed, which agrees with the stress change of -2.46 N/m predicted to accompany formation of 1.5 MLs of coherent Au on Pt(111) from epitaxy theory. The Cu monolayer deposited on Au(111) from an acid sulfate electrolyte was found to be pseudomorphic while the Cu monolayer formed on Au(111) in vacuum was incoherent. The stress-thickness change associated with the coherent monolayer of copper on Au(111) in electrolyte was -0.6 N/m, while conventional epitaxy theories predict a value of +7.76 N/m. STM results elucidated the sulfate adsorption on the copper monolayer caused an expansion of the layer as evidenced by a Moire Structure. For the Cu monolayer on Au(111), the sulfate-induced expansion

  10. Charcoal/Nitrogen Adsorption Cryocooler

    NASA Technical Reports Server (NTRS)

    Bard, Steven

    1987-01-01

    Refrigerator with no wear-related moving parts produces 0.5 W of cooling at 118 K. When fully developed, refrigerator needs no electrical power, and life expectancy of more than 10 yr, operates unattended to cool sensitive infrared detectors for long periods. Only moving parts in adsorption cryocooler are check valves. As charcoal is cooled in canister, gas pressure drops, allowing inlet check valve to open and admit more nitrogen. When canister is heated, pressure rises, closing inlet valve and eventually opening outlet valve.

  11. Moisture adsorption in optical coatings

    NASA Technical Reports Server (NTRS)

    Macleod, H. Angus

    1988-01-01

    The thin film filter is a very large aperture component which is exceedingly useful because of its small size, flexibility and ease of mounting. Thin film components, however, do have defects of performance and especially of stability which can cause problems in systems, particularly where long-term measurements are being made. Of all of the problems, those associated with moisture absorption are the most serious. Moisture absorption occurs in the pore-shaped voids inherent in the columnar structure of the layers. Ion-assisted deposition is a promising technique for substantially reducing moisture adsorption effects in thin film structures.

  12. Hydrogen adsorption on functionalized nanoporous activated carbons.

    PubMed

    Zhao, X B; Xiao, B; Fletcher, A J; Thomas, K M

    2005-05-12

    There is considerable interest in hydrogen adsorption on carbon nanotubes and porous carbons as a method of storage for transport and related energy applications. This investigation has involved a systematic investigation of the role of functional groups and porous structure characteristics in determining the hydrogen adsorption characteristics of porous carbons. Suites of carbons were prepared with a wide range of nitrogen and oxygen contents and types of functional groups to investigate their effect on hydrogen adsorption. The porous structures of the carbons were characterized by nitrogen (77 K) and carbon dioxide (273 K) adsorption methods. Hydrogen adsorption isotherms were studied at 77 K and pressure up to 100 kPa. All the isotherms were Type I in the IUPAC classification scheme. Hydrogen isobars indicated that the adsorption of hydrogen is very temperature dependent with little or no hydrogen adsorption above 195 K. The isosteric enthalpies of adsorption at zero surface coverage were obtained using a virial equation, while the values at various surface coverages were obtained from the van't Hoff isochore. The values were in the range 3.9-5.2 kJ mol(-1) for the carbons studied. The thermodynamics of the adsorption process are discussed in relation to temperature limitations for hydrogen storage applications. The maximum amounts of hydrogen adsorbed correlated with the micropore volume obtained from extrapolation of the Dubinin-Radushkevich equation for carbon dioxide adsorption. Functional groups have a small detrimental effect on hydrogen adsorption, and this is related to decreased adsorbate-adsorbent and increased adsorbate-adsorbate interactions.

  13. Adsorption of beta blockers to environmental surfaces.

    PubMed

    Kibbey, Tohren C G; Paruchuri, Rajiv; Sabatini, David A; Chen, Lixia

    2007-08-01

    Beta-adrenergic blocking agents (beta blockers) are widely used pharmaceuticals which have been detected in the environment. Predicting the transport and ultimate fate of beta blockers in the environment requires understanding their adsorption to soils and sediments, something for which little information is currently available. The objective of this work was to examine the adsorption of three beta blockers, propranolol, metoprolol and nadolol, to a natural alluvial material, as well as to six minerals present as components of the alluvial material. Batch adsorption experiments indicate that, for most of the minerals studied, compound hydrophobicity is an important predictor of adsorption, with propranolol,the most hydrophobic compound studied, adsorbing to the greatest extent. Results further suggest that, for the minerals studied, electrostatic effects are not a good predictor of adsorption; adsorption extent was not well-predicted by either surface zeta potential or by the difference between experiment pH and point of zero charge, despite the cationic nature af the three beta blockers at experiment pH values. Experiments were conducted to examine the effect of an anionic surfactant, sodium dodecyl benzene sulfonate (SDBS), on adsorption. Results indicate that SDBS significantly increases the adsorption of propranolol to two different sorbents. This result is potentially important because surfactants such as SDBS are likely to be present in wastewater effluents with beta blockers and could influence their mobility in the environment.

  14. Polychelated cryogels: hemoglobin adsorption from human blood.

    PubMed

    Erol, Kadir

    2017-02-01

    The separation and purification methods are extremely important for the hemoglobin (Hb) which is a crucial biomolecule. The adsorption technique is popular among these methods and the cryogels have been used quite much due to their macropores and interconnected flow channels. In this study, the Hb adsorption onto the Cu(II) immobilized poly(2-hydroxyethyl methacrylate-glycidyl methacrylate), poly(HEMA-GMA)-Cu(II), cryogels was investigated under different conditions (pH, interaction time, initial Hb concentration, temperature and ionic strength) to optimize adsorption conditions. The swelling test, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscope (SEM), surface area (BET), elemental and ICP-OES analysis were performed for the characterization of cryogels. Polyethyleneimine (PEI) molecule was used as a Cu(II)-chelating ligand. The Hb adsorption capacity of cryogels was determined as 193.8 mg Hb/g cryogel. The isolation of Hb from human blood was also studied under optimum adsorption conditions determined and the Hb (124.5 mg/g cryogel) was isolated. The adsorption model was investigated in the light of Langmuir and Freundlich adsorption isotherm models and it was determined to be more appropriate to the Langmuir adsorption isotherm model.

  15. Arsenate adsorption by unsaturated alluvial sediments

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Arsenate adsorption as a function of solution arsenic concentration and solution pH was investigated on five alluvial sediments from the Antelope Valley, Western Mojave Desert, California. Arsenate adsorption increased with increasing solution pH, exhibited a maximum around pH 4 to 5, and then decr...

  16. BSA adsorption on bimodal PEO brushes.

    PubMed

    Bosker, W T E; Iakovlev, P A; Norde, W; Cohen Stuart, M A

    2005-06-15

    BSA adsorption onto bimodal PEO brushes at a solid surface was measured using optical reflectometry. Bimodal brushes consist of long (N=770) and short (N=48) PEO chains and were prepared on PS surfaces, applying mixtures of PS(29)-PEO(48) and PS(37)-PEO(770) block copolymers and using the Langmuir-Blodgett technique. Pi-A isotherms of (mixtures of) the block copolymers were measured to establish the brush regime. The isotherms of PS(29)-PEO(48) show hysteresis between compression and expansion cycles, indicating aggregation of the PS(29)-PEO(48) upon compression. Mixtures of PS(29)-PEO(48) and PS(37)-PEO(770) demonstrate a similar hysteresis effect, which eventually vanishes when the ratio of PS(37)-PEO(770) to PS(29)-PEO(48) is increased. The adsorption of BSA was determined at brushes for which the grafting density of the long PEO chains was varied, while the total grafting density was kept constant. BSA adsorption onto monomodal PEO(48) and PEO(770) brushes was determined for comparison. The BSA adsorption behavior of the bimodal brushes is similar to the adsorption of BSA at PEO(770) monomodal brushes. The maximum of BSA adsorption at low grafting density of PEO(770) can be explained by ternary adsorption, implying an attraction between BSA and PEO. The contribution of primary adsorption to the total adsorbed amount is negligible.

  17. Ion Exchange and Adsorption of Inorganic Contaminants

    EPA Science Inventory

    In the first part of the chapter, the fundamentals of ion exchange and adsorption processes are explained, with the goal of demonstrating how these principles influence process design for inorganic contaminant removal. In the second part, ion exchange and adsorption processes th...

  18. Phosphoryl functionalized mesoporous silica for uranium adsorption

    NASA Astrophysics Data System (ADS)

    Xue, Guo; Yurun, Feng; Li, Ma; Dezhi, Gao; Jie, Jing; Jincheng, Yu; Haibin, Sun; Hongyu, Gong; Yujun, Zhang

    2017-04-01

    Phosphoryl functionalized mesoporous silica (TBP-SBA-15) was synthesized by modified mesoporous silica with γ-amino propyl triethoxy silane and tributyl phosphate. The obtained samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), small angle X-ray diffraction (SAXRD), thermo-gravimetric/differential thermalanalyzer (TG/DTA), N2 adsorption-desorption (BET) and Fourier transform infrared spectroscopy (FT-IR) techniques. Results showed that TBP-SBA-15 had large surface areas with ordered channel structure. Moreover, the effects of adsorption time, sorbent dose, solution pH, initial uranium concentration and temperature on the uranium adsorption behaviors were investigated. TBP-SBA-15 showed a high uranium adsorption capacity in a broad range of pH values. The U(VI) adsorption rate of TBP-SBA-15 was fast and nearly achieved completion in 10 min with the sorbent dose of 1 g/L. The U(VI) adsorption of TBP-SBA-15 followed the pseudo-second-order kinetic model and Freundlich isotherm model, indicating that the process was belonged to chemical adsorption. Furthermore, the thermodynamic parameters (ΔG0, ΔH0 and ΔS0) confirmed that the adsorption process was endothermic and spontaneous.

  19. 9-Hydroxypiperitone beta-D-glucopyranoside and other polar constituents from dill (Anethum graveolens L.) herb.

    PubMed

    Bonnländer, B; Winterhalter, P

    2000-10-01

    A methanolic extract from dill (Anethum graveolens) herb was subjected to XAD-2 adsorption chromatography. The methanolic eluate was fractionated with the all liquid chromatographic technique of multilayer coil countercurrent chromatography (MLCCC). After acetylation of MLCCC subfractions and flash chromatography, final purification of dill herb constituents was achieved by preparative and/or analytical HPLC. Nine compounds were obtained in pure form, including the beta-D-glucopyranosides of 9-hydroxypiperitone, p-menth-2-ene-1,6-diol, and 8-hydroxygeraniol. Structure elucidation is based on electrospray ionization ion trap multiple mass spectrometry (ESI-MS/MS) as well as one- and two-dimensional nuclear magnetic resonance spectroscopy.

  20. How Surface Heterogeneity Affects Protein Adsorption: Annealing of OTS Patterns and Albumin Adsorption Kinetics*

    PubMed Central

    Hodgkinson, Gerald N.; Hlady, Vladimir

    2009-01-01

    Fluorescence microscopy and intensity histogram analysis techniques were used to monitor spatially-resolved albumin adsorption kinetics to model heterogeneous surfaces on sub-μm scales. Several distinct protein subpopulations were resolved, each represented by a normal distribution of adsorption densities on the adsorbent surface. Histogram analyses provided dynamic information of mean adsorption density, spread in adsorption density, and surface area coverage for each distinct protein subpopulation. A simple adsorption model is proposed in which individual protein binding events are predicted by the summation of multiple protein's surface sub-site interactions with different binding energy sub-sites on adsorbent surfaces. This model is predictive of the albumin adsorption on the patterns produced by one step μ-contact printing (μCP) of octadecyltrichlorosilane (OTS) on glass but fails to describe adsorption once the same patterns are altered by a thermal annealing step. PMID:19746205

  1. A "stripping" ligand tactic for use with the kinetic locking-on strategy: its use in the resolution and bioaffinity chromatographic purification of NAD(+)-dependent dehydrogenases.

    PubMed

    O'Flaherty, M; O'Carra, P; McMahon, M; Mulcahy, P

    1999-08-01

    The kinetic locking-on strategy utilizes soluble analogues of the target enzymes' specific substrate to promote selective adsorption of individual NAD(+)-dependent dehydrogenases on their complementary immobilized cofactor derivative. Application of this strategy to the purification of NAD(+)-dependent dehydrogenases from crude extracts has proven that it can yield bioaffinity systems capable of producing one-chromatographic-step purifications with yields approaching 100%. However, in some cases the purified enzyme preparation was found to be contaminated with other proteins weakly bound to the immobilized cofactor derivative through binary complex formation and/or nonspecific interactions, which continuously "dribbled" off the matrix during the chromatographic procedure. The fact that this problem can be overcome by including a short pulse of 5'-AMP (stripping ligand) in the irrigant a couple of column volumes prior to the discontinuation of the specific substrate analogue (locking-on ligand) is clear from the results presented in this report. The general effectiveness of this auxiliary tactic has been assessed using model studies and through incorporation into an actual purification from a crude cellular extract. The results confirm the usefulness of the stripping-ligand tactic for the resolution and purification of NAD(+)-dependent dehydrogenases when using the locking-on strategy. These studies have been carried out using bovine liver glutamate dehydrogenase (GDH, EC 1.4.1.3), yeast alcohol dehydrogenase (YADH, EC 1.1.1.1), porcine heart mitochondrial malate dehydrogenase (mMDH, EC 1.1.1.37), and bovine heart L-lactate dehydrogenase (l-LDH, EC 1.1.1.27).

  2. Factors affecting drug adsorption on beta zeolites.

    PubMed

    Pasti, Luisa; Sarti, Elena; Cavazzini, Alberto; Marchetti, Nicola; Dondi, Francesco; Martucci, Annalisa

    2013-05-01

    The adsorption behaviour of three commonly used drugs, namely ketoprofen, hydrochlorothiazide and atenolol, from diluted aqueous solutions on beta zeolites with different SiO2/Al2O3 ratio (i.e. 25, 38 and 360) was investigated by changing the ionic strength and the pH, before and after thermal treatment of the adsorbents. The selective adsorption of drugs was confirmed by thermogravimetry and X-ray diffraction. The adsorption capacity of beta zeolites was strongly dependent on both the solution pH and the alumina content of the adsorbent. Such a remarkable difference was interpreted as a function of the interactions between drug molecules and zeolite surface functional groups. Atenolol was readily adsorbed on the less hydrophobic zeolite, under pH conditions in which electrostatic interactions were predominant. On the other hand, ketoprofen adsorption was mainly driven by hydrophobic interactions. For undissociated molecules the adsorption capability increased with the increase of hydrophobicity.

  3. Adsorption and desorption of reversible supramolecular polymers

    NASA Astrophysics Data System (ADS)

    Zweistra, Henk J. A.; Besseling, N. A. M.

    2006-08-01

    We report numerical mean-field results on the quasichemical level of approximation that describe adsorption of reversible supramolecular polymers at a flat interface. Emphasis is laid on the regime of strong adsorption from a dilute solution. There are two differences with respect to macromolecular polymer adsorption: (i) adsorption sets in at relatively high monomer concentrations of the surrounding solution, and (ii) the surface is filled within a much narrower concentration range. Contrary to macromolecular polymers, supramolecular polymers can therefore be desorbed by dilution of the equilibrium solution by solvent within an experimentally accessible concentration window. Based on simple thermodynamic arguments, we provide a quantitative explanation why supramolecular polymers adsorb at relatively high concentrations. Moreover, we discuss the (by comparison) narrow concentration window wherein filling of the surface occurs. This is attributed to the cooperative nature of supramolecular polymer adsorption. The degree of cooperativity is quantified by means of the Hill parameter n .

  4. Adsorption of xenon and krypton on shales

    NASA Technical Reports Server (NTRS)

    Podosek, F. A.; Bernatowicz, T. J.; Kramer, F. E.

    1981-01-01

    A method that uses a mass spectrometer as a manometer is employed in the measurement of Xe and Kr adsorption parameters on shales and related samples, where gas partial pressures were lower than 10 to the -11th atm, corresponding adsorption coverages are only small fractions of a monolayer, and Henry's Law behavior is expected and observed. Results show heats of adsorption in the 2-7 kcal/mol range, and Henry constants at 0-25 C of 1 cu cm STP/g per atmosphere are extrapolated. Although the adsorption properties obtained are variable by sample, the range obtained suggests that shales may be capable of an equilibrium adsorption with modern air high enough to account for a significant fraction of the atmospheric inventory of Xe, and perhaps even of Kr. This effect will nevertheless not account for the factor-of-25 defficiency of atmospheric Xe, in comparison with the planetary gas patterns observed in meteorites.

  5. [A peak recognition algorithm designed for chromatographic peaks of transformer oil].

    PubMed

    Ou, Linjun; Cao, Jian

    2014-09-01

    In the field of the chromatographic peak identification of the transformer oil, the traditional first-order derivative requires slope threshold to achieve peak identification. In terms of its shortcomings of low automation and easy distortion, the first-order derivative method was improved by applying the moving average iterative method and the normalized analysis techniques to identify the peaks. Accurate identification of the chromatographic peaks was realized through using multiple iterations of the moving average of signal curves and square wave curves to determine the optimal value of the normalized peak identification parameters, combined with the absolute peak retention times and peak window. The experimental results show that this algorithm can accurately identify the peaks and is not sensitive to the noise, the chromatographic peak width or the peak shape changes. It has strong adaptability to meet the on-site requirements of online monitoring devices of dissolved gases in transformer oil.

  6. Reversed-phase liquid chromatographic separation and simultaneous profiling of steroidal glycoalkaloids and their aglycones.

    PubMed

    Kuronen, P; Väänänen, T; Pehu, E

    1999-11-19

    Improved and simplified reversed-phase liquid chromatographic conditions for the separation and simultaneous profiling of both steroidal glycoalkaloids and their aglycones, having solanidane- or spirosolane-type structures, are described. The most reproducible retention behavior for these ionizable compounds on C18 columns was achieved under isocratic and gradient elution conditions using acetonitrile in combination with triethylammonium phosphate buffer at pH 3.0, when basic functional groups of solutes and silanol groups on the silica are fully protonated minimizing ionic interactions. Gradient elution was the only feasible approach for the simultaneous separation of steroidal glycoalkaloids and their aglycones. A Zorbax SB C18 column, specially designed for low-pH separations, showed good performance in critical separations. The impurities of the commercial tomatine and tomatidine standards were studied and confirmed using mass spectrometric, liquid chromatographic and thin-layer chromatographic methods.

  7. A new concept for variance analysis of hyphenated chromatographic data avoiding signal warping.

    PubMed

    Zerzucha, Piotr; Kazura, Małgorzata; de Beer, Dalene; Joubert, Elizabeth; Schulze, Alexandra E; Beelders, Theresa; de Villiers, André; Walczak, Beata

    2013-05-24

    Analysis of variance of chromatographic data is usually performed on the peak table or on entire chromatograms. These two data forms require signal pretreatment. Peak table requires peak detection, their standards and quantification, and the second form of data organization requires warping of the studied chromatograms to eliminate the observed peak shifts, which occurs due to minor variations in chromatographic conditions. In our study, a new form of data representation well suited for chromatographic data originating from multi-channel detection is proposed. It requires neither warping of chromatograms, nor peak detection. Its principles and performance are demonstrated for a real data set (being a part of a larger research project initiated to characterize the infusion of fermented rooibos herbal tea in terms of phenolic composition and antioxidant activity). As the method of choice for the analysis of data variation, the Multiple Analysis of Variance applied to the pairwise data representation was chosen.

  8. Chromatographic immunoassays: strategies and recent developments in the analysis of drugs and biological agents

    PubMed Central

    Matsuda, Ryan; Rodriguez, Elliott; Suresh, Doddavenkatanna; Hage, David S

    2015-01-01

    A chromatographic immunoassay is a technique in which an antibody or antibody-related agent is used as part of a chromatographic system for the isolation or measurement of a specific target. Various binding agents, detection methods, supports and assay formats have been developed for this group of methods, and applications have been reported that range from drugs, hormones and herbicides to peptides, proteins and bacteria. This review discusses the general principles and applications of chromatographic immunoassays, with an emphasis being given to methods and formats that have been developed for the analysis of drugs and biological agents. The relative advantages or limitations of each format are discussed. Recent developments and research in this field, as well as possible future directions, are also considered. PMID:26571109

  9. Simultaneous high-performance liquid chromatographic determination of suxibuzone and its metabolites in plasma and urine.

    PubMed

    Marunaka, T; Shibata, T; Minami, Y; Umeno, Y; Shindo, T

    1980-11-01

    A high-performance liquid chromatographic method is described for the simultaneous determination of the anti-inflammatory agent suxibuzone and its metabolites, 4-hydroxymethylphenylbutazone, phenylbutazone, oxyphenbutazone, and gamma-hydroxyphenylbutazone, in plasma and urine. Acidified plasma or urine is extracted with benzenecyclohexane (1:1). The organic extract is reduced to dryness and the resulting residue is redissolved in methanol. Aliquots of this solution are chromatographed on a reversed-phase column using a mobile phase of methanol--0.5 M KH2PO4 (linear gradient from 0 to 100% methanol at 8% min with a flow rate of 2.0 ml/min) on a high-performance liquid chromatograph equipped with a UV absorbance detector (254 nm). Detection is limited to 0.10 microgram/ml for suxibuzone and 4-hydroxymethylphenylbutazone and to 0.05 microgram/ml for the other metabolites.

  10. Micro and nanotechnologies for the development of an integrated chromatographic system

    NASA Astrophysics Data System (ADS)

    Casals, O.; Romano-Rodríguez, A.; Illa, X.; Zamani, C.; Vilà, A.; Morante, J. R.; Gràcia, I.; Ivanov, P.; Sabaté, N.; Fonseca, L.; Santander, J.; Figueras, E.; Cané, C.

    2007-05-01

    The development of an integrated gas chromatographic system using micro and nanotechnologies is presented in this paper. For this purpose, the different components of the chromatographic system, namely the preconcentrator, the chromatographic column and the gas sensors are being investigated and developed, and the actual state of this investigation is presented. The proposed target application comes from the agrofood industry, in particular the determination of the fish freshness. The structure of the preconcentrator has been fabricated using deep reactive ion etching (DRIE). The same fabrication technique has been employed for the patterning of the silicon microcolumns, which have been sealed with Pyrex glass. Inlet and outlets have been connected and initial experiments of functionalization have been performed. Gas sensors have been obtained by microdeposition of doped WO 3 or SnO II nanomaterials on microhotplates and their responses to the gases of interest have been measured, proving that the target gas concentrations can be detected.

  11. Comparison of three liquid chromatographic methods for egg-white protein analysis.

    PubMed

    Awadé, A C; Efstathiou, T

    1999-02-19

    This paper describes and compares three chromatographic methods for the analysis of egg-white proteins. Gel-permeation chromatography allowed the separation of seven peaks from egg white, with an almost total protein recovery. A clean separation of ovomucin and lysozyme from the bulk of the proteins was obtained with this method. Reversed-phase high-performance liquid chromatography led to the fractionation of at least eight peaks. With this chromatographic method, the recovery was relatively poor. Approximately 30% of the ovalbumin was retained in the column after the elution. Finally, eleven chromatographic peaks were separated from egg white by high-performance liquid chromatography on an anion-exchange column. The recovery of proteins was almost total. The latter method afforded higher resolution.

  12. Enhanced purity, activity and structural integrity of yeast ribosomes purified using a general chromatographic method.

    PubMed

    Leshin, Jonathan A; Rakauskaitė, Rasa; Dinman, Jonathan D; Meskauskas, Arturas

    2010-01-01

    One of the major challenges facing researchers working with eukaryotic ribosomes lies in their lability relative to their eubacterial and archael counterparts. In particular, lysis of cells and purification of eukaryotic ribosomes by conventional differential ultracentrifugation methods exposes them for long periods of time to a wide range of co-purifying proteases and nucleases, negatively impacting their structural integrity and functionality. A chromatographic method using a cysteine charged Sulfolink resin was adapted to address these problems. This fast and simple method significantly reduces co-purifying proteolytic and nucleolytic activities, producing good yields of highly biochemically active yeast ribosomes with fewer nicks in their rRNAs. In particular, the chromatographic purification protocol significantly improved the quality of ribosomes isolated from mutant cells. This method is likely applicable to mammalian ribosomes as well. The simplicity of the method, and the enhanced purity and activity of chromatographically purified ribosome represents a significant technical advancement for the study of eukaryotic ribosomes.

  13. Preparation of dye-ligand affinity chromatographic packings based on monodisperse poly(glycidylmethacrylate-co-ethylenedimethacrylate) beads and their chromatographic properties.

    PubMed

    Wu, Feiyan; Zhu, Yan; Jia, Zhishen

    2006-11-17

    Monodisperse porous particles, poly(glycidylmethacrylate-co-ethylenedimethacrylate), P(GMA-EDMA) beads with diameter of 7 microm were prepared by a single-step swelling and polymerization method. The polymer particles were advantaged through immobilization of Procion Bule MX-R, which was incubated by epichlorohydrin via the epoxide groups on the particles surface. The Procion Bule MX-R-immobilized P(GMA-EDMA) beads were mechanically stable and acted as the rigid matrix for column chromatography in HPLC mode. The chromatographic properties of the dye-ligand affinity chromatographic stationary phase for biopolymers separation are discussed. This affinity column has advantages of enabling biopolymer separation, high efficiency and low backpressure. Lysozyme and BSA were fast separated within 10min using this affinity column. The column was also used for the purification of lysozyme from chicken egg white.

  14. Temperature Swing Adsorption Compressor Development

    NASA Technical Reports Server (NTRS)

    Finn, John E.; Mulloth, Lila M.; Affleck, Dave L.

    2001-01-01

    Closing the oxygen loop in an air revitalization system based on four-bed molecular sieve and Sabatier reactor technology requires a vacuum pump-compressor that can take the low-pressure CO, from the 4BMS and compress and store for use by a Sabatier reactor. NASA Ames Research Center proposed a solid-state temperature-swing adsorption (TSA) compressor that appears to meet performance requirements, be quiet and reliable, and consume less power than a comparable mechanical compressor/accumulator combination. Under this task, TSA compressor technology is being advanced through development of a complete prototype system. A liquid-cooled TSA compressor has been partially tested, and the rest of the system is being fabricated. An air-cooled TSA compressor is also being designed.

  15. Derivatization in gas chromatographic determination of phenol and aniline traces in aqueous media

    NASA Astrophysics Data System (ADS)

    Gruzdev, I. V.; Zenkevich, I. G.; Kondratenok, B. M.

    2015-06-01

    Substituted anilines and phenols are the most common hydrophilic organic environmental toxicants. The principles of gas chromatographic determination of trace amounts of these compounds in aqueous media at concentrations <=0.1 μg litre-1 based on synthesis of their derivatives (derivatization) directly in the aqueous phase are considered. Conversion of relatively hydrophilic analytes into more hydrophobic derivatives makes it possible to achieve such low detection limits and optimize the protocols of extractive preconcentration and selective chromatographic detection. Among the known reactions, this condition is best met by electrophilic halogenation of compounds at the aromatic moiety. The bibliography includes 177 references.

  16. Fermentation condition outweighed truffle species in affecting volatile organic compounds analyzed by chromatographic fingerprint system.

    PubMed

    Tang, Ya-Jie; Wang, Guan; Li, Yuan-Yuan; Zhong, Jian-Jiang

    2009-08-04

    The influences of fermentation conditions and truffle species (i.e., Tuber melanosporum, Tuber sinense, Tuber indicum, and Tuber aestivum) on the volatile organic compounds (VOCs) originated from truffle fermentation mycelia were studied by using chromatographic fingerprint system for the first time. Gas chromatography combined with statistical methods including similarity analysis and hierarchical cluster analysis was applied to develop chromatographic fingerprint system for truffle VOCs evaluation. Fermentation conditions affected the VOCs from truffle fermentation mycelia much more significantly than truffle species. This indicated that it is possible to adjust the aroma of truffle fermentation mycelia similar with the natural fruiting-body through the control of fermentation process.

  17. Chromatographic determination of the diffusion coefficients of light hydrocarbons in polymers

    NASA Astrophysics Data System (ADS)

    Yakubenko, E. E.; Korolev, A. A.; Chapala, P. P.; Bermeshev, M. V.; Kanat'eva, A. Yu.; Kurganov, A. A.

    2017-01-01

    Gas-chromatographic determination of the diffusion coefficients that allows for the compressibility of the mobile phase has been suggested. The diffusion coefficients were determined for light hydrocarbons C1-C4 in four polymers with a high free volume, which are candidates for use as gas-separating membranes. The diffusion coefficients calculated from chromatographic data were shown to be one or two orders of magnitude smaller than the values obtained by the membrane method. This may be due to the presence of an additional flow through the membrane caused by the pressure gradient across the membrane in membrane methods.

  18. Quantitative high-performance liquid chromatographic determination of acrolein in plasma after derivatization with Luminarin 3.

    PubMed

    Paci, A; Rieutord, A; Guillaume, D; Traoré, F; Ropenga, J; Husson, H P; Brion, F

    2000-03-10

    A rapid, sensitive and specific high-performance liquid chromatographic method for the quantification of acrolein (1), one of the toxic metabolites of oxazaphosphorine alkylating agents (cyclophosphamide and ifosfamide) was developed. Condensation of acrolein with Luminarin 3 afforded a fluorescent derivative that could be specifically detected and quantified. Chromatographic conditions involved a C18 RP column Uptisphere and a gradient elution system to optimize resolution and time analysis. The method showed high sensitivity with a limit of detection of 100 pmol/ml and a limit of quantification of 300 pmol/ml. This technique is particularly suitable for pharmacokinetic studies on plasma of oxazaphosphorine-receiving patients.

  19. Determination of Cr(III) in chromic acid. Comparison of spectrophotometric and ion chromatographic methods

    SciTech Connect

    Smith, R.E.; Smith, C.H.

    1986-04-01

    Two methods have been developed for determining Cr(III) in chromic acid solutions. Both methods are based on the formation of a Cr-EDTA complex. The ion chromatographic method detects the Cr-EDTA as an anion using chemically suppressed conductivity. The spectrophotometric method detects the Cr-EDTA as a colored complex by measuring the absorbance at 540 nm. The conditions necessary for forming the Cr-EDTA complex are described. The results obtained by the spectrophotometric and ion chromatographic methods are compared. 15 refs., 5 figs., 1 tab.

  20. Surfactant modified/mediated thin-layer chromatographic systems for the analysis of amino acids.

    PubMed

    Bhawani, Showkat A; Albishri, Hassan M; Khan, Ziya Ahmad; Mohamad Ibrahim, Mohamad N; Mohammad, A

    2013-01-01

    This review incorporates a large number of chromatographic systems modified by the surfactants. A large number of solvent systems and stationary phases are summarized in this paper. Three different kinds of surfactants (anionic, cationic, and nonionic) are used as modifiers for stationary phases as well as solvent systems. Surfactants are used at all the three different concentration levels (below, above, and at critical micelle concentration) where surfactants behave differently. Modifications of both stationary phases and solvent systems by surfactants produced a new generation of chromatographic systems. Microemulsion solvent systems are also incorporated in this paper. Microemulsion thin-layer chromatography is a new approach in the field of chromatography.

  1. Surfactant Modified/Mediated Thin-Layer Chromatographic Systems for the Analysis of Amino Acids

    PubMed Central

    Bhawani, Showkat A.; Albishri, Hassan M.; Mohamad Ibrahim, Mohamad N.; Mohammad, A.

    2013-01-01

    This review incorporates a large number of chromatographic systems modified by the surfactants. A large number of solvent systems and stationary phases are summarized in this paper. Three different kinds of surfactants (anionic, cationic, and nonionic) are used as modifiers for stationary phases as well as solvent systems. Surfactants are used at all the three different concentration levels (below, above, and at critical micelle concentration) where surfactants behave differently. Modifications of both stationary phases and solvent systems by surfactants produced a new generation of chromatographic systems. Microemulsion solvent systems are also incorporated in this paper. Microemulsion thin-layer chromatography is a new approach in the field of chromatography. PMID:24455427

  2. Host cell protein adsorption characteristics during protein A chromatography.

    PubMed

    Tarrant, Richard D R; Velez-Suberbie, M Lourdes; Tait, Andrew S; Smales, C Mark; Bracewell, Daniel G

    2012-07-01

    Protein A chromatography is a critical and 'gold-standard' step in the purification of monoclonal antibody (mAb) products. Its ability to remove >98% of impurities in a single step alleviates the burden on subsequent process steps and facilitates the implementation of platform processes, with a minimal number of chromatographic steps. Here, we have evaluated four commercially available protein A chromatography matrices in terms of their ability to remove host cell proteins (HCPs), a complex group of process related impurities that must be removed to minimal levels. SELDI-TOF MS was used as a screening tool to generate an impurity profile fingerprint for each resin and indicated a number of residual impurities present following protein A chromatography, agreeing with HCP ELISA. Although many of these were observed for all matrices there was a significantly elevated level of impurity binding associated with the resin based on controlled pore glass under standard conditions. Use of null cell line supernatant with and without spiked purified mAb demonstrated the interaction of HCPs to be not only with the resin back-bone but also with the bound mAb. A null cell line column overload and sample enrichment method before 2D-PAGE was then used to determine individual components associated with resin back-bone adsorption. The methods shown allow for a critical analysis of HCP removal during protein A chromatography. Taken together they provide the necessary process understanding to allow process engineers to identify rational approaches for the removal of prominent HCPs.

  3. Adsorption of water vapor by poly(styrenesulfonic acid), sodium salt: isothermal and isobaric adsorption equilibria.

    PubMed

    Toribio, F; Bellat, J P; Nguyen, P H; Dupont, M

    2004-12-15

    Air conditioning and dehumidifying systems based on sorption on solids are of great interest, especially in humid climates, because they allow reduction of thermal loads and use of chlorofluorocarbons. Previous studies have shown that hydrophilic polymers such as sulfonic polymers can have very high performance in water adsorption from air. The aim of this study was to characterize the water vapor adsorption properties of fully sulfonated and monosulfonated poly(styrenesulfonic acid), sodium salt, and to elucidate the mechanism of adsorption on these materials. Adsorption isotherms have been determined by TGA between 298 and 317 K for pressures ranging from 0.1 to 45 hPa. They have type II of the IUPAC classification and a small hysteresis loop between adsorption and desorption processes was observed only for the monosulfonated sample. Water content is up to 80% weight at 80% relative humidity. Adsorption isotherms have been well fitted with the FHH model. Adsorption-desorption isobars have been determined by TGA under 37 hPa in the temperature range 298-373 K. They show that these polymers can be completely regenerated by heating at 313 K under humidified air. No degradation of the adsorption properties has been observed after several regenerations. Adsorption enthalpies and entropies have been deduced from the Clapeyron equation and from DSC measurements. A good agreement was found. A mechanism of adsorption is proposed considering two kinds of adsorbate: bounded water in electrostatic interaction with functional groups and free water resulting from condensation.

  4. Modeling the adsorption of mixed gases based on pure gas adsorption properties

    NASA Astrophysics Data System (ADS)

    Tzabar, N.; Holland, H. J.; Vermeer, C. H.; ter Brake, H. J. M.

    2015-12-01

    Sorption-based Joule-Thomson (JT) cryocoolers usually operate with pure gases. A sorption-based compressor has many benefits; however, it is limited by the pressure ratios it can provide. Using a mixed-refrigerant (MR) instead of a pure refrigerant in JT cryocoolers allows working at much lower pressure ratios. Therefore, it is attractive using MRs in sorption- based cryocoolers in order to reduce one of its main limitations. The adsorption of mixed gases is usually investigated under steady-state conditions, mainly for storage and separation processes. However, the process in a sorption compressor goes through various temperatures, pressures and adsorption concentrations; therefore, it differs from the common mixed gases adsorption applications. In order to simulate the sorption process in a compressor a numerical analysis for mixed gases is developed, based on pure gas adsorption characteristics. The pure gas adsorption properties have been measured for four gases (nitrogen, methane, ethane, and propane) with Norit-RB2 activated carbon. A single adsorption model is desired to describe the adsorption of all four gases. This model is further developed to a mixed-gas adsorption model. In future work more adsorbents will be tested using these four gases and the adsorption model will be verified against experimental results of mixed-gas adsorption measurements.

  5. Competitive ion-exchange adsorption of proteins: competitive isotherms with controlled competitor concentration.

    PubMed

    Cano, Tony; Offringa, Natalie D; Willson, Richard C

    2005-06-24

    The competitive adsorption processes inevitably present in chromatographic separations of complex mixtures have not been extensively studied. This is partly due to the difficulty of measuring true competitive isotherms, in which all system parameters (including competitor concentrations) are held constant. We report a novel approach to determining competitive protein adsorption isotherms in which the competitor concentration is held constant across the entire isotherm. By using the heme prosthetic group in cytochrome b5 as a quantitative spectrophotometric label, competitive isotherms between cytochrome b5 and alpha-lactalbumin can be constructed. Similarly, manganese-substituted protoporphyrin IX heme replacement allows the non-perturbing labeling of individual cytochrome b5 conservative surface charge mutants by replacement of a single atom in the interior of the protein. This labeling allows the study of competition between cytochrome b5 charge mutants of identical size and shape, which differ only in charge arrangement. Using these techniques, the effect of competing species on equilibrium behavior and the apparent heterogeneity of anion-exchange adsorbents in the presence of competitors can be quantitatively studied by fitting the data to two popular single-component binding models, the Temkin and the Langmuir-Freundlich (L-F) isotherms.

  6. Determination of competitive adsorption isotherms applying the nonlinear frequency response method. Part II. Experimental demonstration.

    PubMed

    Ilić, Milica; Petkovska, Menka; Seidel-Morgenstern, Andreas

    2009-08-14

    This paper demonstrates an experimental application of the nonlinear frequency response (FR) method extension to determine adsorption isotherms of binary mixtures. This method, based on the analysis of the response of a chromatographic column subjected to the sinusoidal inlet concentration changes, is shown to be an alternative for isotherm determination. The critical issue related to the successful application of the method is to reach experimentally the low frequency asymptotic behaviour of the corresponding frequency response functions (FRFs). Although, there are different possibilities to perform periodical inlet concentration changes, in this paper only simultaneous changes for both components were considered. The adsorption of phenol and 2-phenylethanol on octadecyl silica was analyzed experimentally using a mixture of methanol and water as a solvent. Parameters of competitive isotherms were also estimated for comparison using the classical perturbation method. Despite certain differences between competitive isotherms estimated with the two methods that were found, the obtained results show the potential of the nonlinear FR method for measuring competitive isotherms.

  7. Arsenic Adsorption Equilibrium Concentration and Adsorption Rate of Activated Carbon Coated with Ferric-Aluminum Hydroxides

    NASA Astrophysics Data System (ADS)

    Zhang, M.; Sugita, H.; Oguma, T.; Hara, J.; Takahashi, S.

    2015-12-01

    In some areas of developing countries, ground or well water contaminated with arsenic has been reluctantly used as drinking water. It is highly desirable that effective and inexpensive arsenic removal agents should be developed and provided to reduce the potential health risk. Previous studies demonstrated that activated carbon coated with ferric-aluminum hydroxides (Fe-Al-C) has high adsorptive potential for removal of arsenic. In this study, a series of experiments using Fe-Al-C were carried to discuss adsorption equilibrium time, adsorption equilibrium concentration and adsorption rate of arsenic for Fe-Al-C. Fe-Al-C used in this study was provided by Astec Co., Ltd. Powder reagent of disodium hydrogen arsenate heptahydrate was dissolved into ion-exchanged water. The solution was then further diluted with ion-exchanged water to be 1 and 10 mg/L as arsenic concentration. The pH of the solution was adjusted to be around 7 by adding HCl and/or NaOH. The solution was used as artificial arsenic contaminated water in two types of experiments (arsenic adsorption equilibrium and arsenic adsorption rate tests). The results of the arsenic equilibrium tests were showed that a time period of about 3 days to reach apparent adsorption equilibrium for arsenic. The apparent adsorption equilibrium concentration and adsorbed amount of arsenic on Fe-Al-C adsorbent could be estimated by application of various adsorption isotherms, but the distribution coefficient of arsenic between solid and liquid varies with experimental conditions such as initial concentration of arsenic and addition concentration of adsorbent. An adsorption rate equation that takes into account the reduction in the number of effective adsorption sites on the adsorbent caused by the arsenic adsorption reaction was derived based on the data obtained from the arsenic adsorption rate tests.

  8. Monte Carlo simulations of Protein Adsorption

    NASA Astrophysics Data System (ADS)

    Sharma, Sumit; Kumar, Sanat K.; Belfort, Georges

    2008-03-01

    Amyloidogenic diseases, such as, Alzheimer's are caused by adsorption and aggregation of partially unfolded proteins. Adsorption of proteins is a concern in design of biomedical devices, such as dialysis membranes. Protein adsorption is often accompanied by conformational rearrangements in protein molecules. Such conformational rearrangements are thought to affect many properties of adsorbed protein molecules such as their adhesion strength to the surface, biological activity, and aggregation tendency. It has been experimentally shown that many naturally occurring proteins, upon adsorption to hydrophobic surfaces, undergo a helix to sheet or random coil secondary structural rearrangement. However, to better understand the equilibrium structural complexities of this phenomenon, we have performed Monte Carlo (MC) simulations of adsorption of a four helix bundle, modeled as a lattice protein, and studied the adsorption behavior and equilibrium protein conformations at different temperatures and degrees of surface hydrophobicity. To study the free energy and entropic effects on adsorption, Canonical ensemble MC simulations have been combined with Weighted Histogram Analysis Method(WHAM). Conformational transitions of proteins on surfaces will be discussed as a function of surface hydrophobicity and compared to analogous bulk transitions.

  9. Functionalized SBA-15 materials for bilirubin adsorption

    NASA Astrophysics Data System (ADS)

    Tang, Tao; Zhao, Yanling; Xu, Yao; Wu, Dong; Xu, Jun; Deng, Feng

    2011-05-01

    To investigate the driving force for bilirubin adsorption on mesoporous materials, a comparative study was carried out between pure siliceous SBA-15 and three functionalized SBA-15 mesoporous materials: CH 3-SBA-15 (MS), NH 2-SBA-15 (AS), and CH 3/NH 2-SBA-15 (AMS) that were synthesized by one-pot method. The obtained materials exhibited large surface areas (553-810 m 2/g) and pore size (6.6-7.1 nm) demonstrated by XRD and N 2-ad/desorption analysis. The SEM images showed that the materials had similar fiberlike morphology. The functionalization extent was calculated according to 29Si MAS NMR spectra and it was close to the designed value (10%). The synthesized mesoporous materials were used as bilirubin adsorbents and showed higher bilirubin adsorption capacities than the commercial active carbon. The adsorption capacities of amine functionalized samples AMS and AS were larger than those of pure siliceous SBA-15 and MS, indicating that electrostatic interaction was the dominant driving force for bilirubin adsorption on mesoporous materials. Increasing the ionic strength of bilirubin solution by adding NaCl would decrease the bilirubin adsorption capacity of mesoporous material, which further demonstrated that the electrostatic interaction was the dominant driving force for bilirubin adsorption. In addition, the hydrophobic interaction provided by methyl groups could promote the bilirubin adsorption.

  10. ENVIRONMENTAL TECHNOLOGY VERIFICATION REPORT, EXPLOSIVES DETECTION TECHNOLOGY, SRI INSTRUMENTS, MODEL 8610C, GAS CHROMATOGRAPH/THERMIONIC IONIZATION DETECTION

    EPA Science Inventory

    The SRI Model 86 1 OC gas chromatograph (GC) is a transportable instrument that can provide on-site analysis of soils for explosives. Coupling this transportable gas chromatograph with a thermionic ionization detector (TID) allows for the determination of explosives in soil matri...

  11. Characterization of Gas Chromatographic Liquid Phases Using McReynolds Constants. An Experiment for Instrumental Analysis Laboratory.

    ERIC Educational Resources Information Center

    Erskine, Steven R.; And Others

    1986-01-01

    Describes a laboratory experiment that is designed to aid in the understanding of the fundamental process involved in gas chromatographic separations. Introduces the Kovats retention index system for use by chemistry students to establish criteria for the optimal selection of gas chromatographic stationary phases. (TW)

  12. Adsorption of amylase enzyme on ultrafiltration membranes.

    PubMed

    Beier, Søren Prip; Enevoldsen, Ann Dorrit; Kontogeorgis, Georgios M; Hansen, Ernst B; Jonsson, Gunnar

    2007-08-28

    A method to measure the static adsorption on membrane surfaces has been developed and described. The static adsorption of amylase-F has been measured on two different ultrafiltration membranes, both with a cutoff value of 10 kDa (a PES membrane and the ETNA10PP membrane, which is a surface-modified PVDF membrane). The adsorption follows the Langmuir adsorption theory. Thus, the static adsorption consists of monolayer coverage and is expressed both as a permeability drop and an adsorption resistance. From the adsorption isotherms, the maximum static permeability drops and the maximum static adsorption resistances are determined. The maximum static permeability drop for the hydrophobic PES membrane is 75%, and the maximum static adsorption resistance is 0.014 m2.h.bar/L. The maximum static permeability drop for the hydrophilic surface-modified PVDF membrane (ETNA10PP) is 23%, and the maximum static adsorption resistance is 0.0046 m2.h.bar/L. The difference in maximum static adsorption, by a factor of around 3, affects the performance during the filtration of a 5 g/L amylase-F solution at 2 bar. The two membranes behave very similarly during filtration with almost equal fluxes and retentions even though the initial water permeability of the PES membrane is around 3 times larger than the initial water permeability of the ETNA10PP membrane. This is mainly attributed to the larger maximum static adsorption of the PES membrane. The permeability drop during filtration exceeds the maximum static permeability drop, indicating that the buildup layer on the membranes during filtration exceeds monolayer coverage, which is also seen by the increase in fouling resistance during filtration. The accumulated layer on the membrane surface can be described as a continually increasing cake-layer thickness, which is independent of the membrane type. At higher concentrations of enzyme, concentration polarization effects cannot be neglected. Therefore, stagnant film theory and the osmotic

  13. Apparatus for the study of macromolecular adsorption

    NASA Astrophysics Data System (ADS)

    Mayo, C. S.; Hallock, R. B.

    1989-04-01

    A surface plasmon adsorbate monitor (SPAM) is described which allows the adsorption of macromolecules or other adsorbates to a metal surface to be monitored. Surface plasmons are employed and the apparatus has no moving parts. The kinetics of adsorption may be studied on a time scale of seconds rather than the more common time scale of minutes; a simple improvement in computer memory access should allow temporal studies in the millisecond range. As an illustration, the adsorption of carboxyl-terminated polystyrene from a solution with acetone onto a silver surface is measured.

  14. Adsorption of lead over graphite oxide.

    PubMed

    Olanipekun, Opeyemi; Oyefusi, Adebola; Neelgund, Gururaj M; Oki, Aderemi

    2014-01-24

    The adsorption efficiency and kinetics of removal of lead in presence of graphite oxide (GO) was determined using the Atomic Absorption Spectrophotometer (AAS). The GO was prepared by the chemical oxidation of graphite and characterized using FTIR, SEM, TGA and XRD. The adsorption efficiency of GO for the solution containing 50, 100 and 150 ppm of Pb(2+) was found to be 98%, 91% and 71% respectively. The adsorption ability of GO was found to be higher than graphite. Therefore, the oxidation of activated carbon in removal of heavy metals may be a viable option to reduce pollution in portable water.

  15. A novel method for the determination of adsorption partition coefficients of minor gases in a shale sample by headspace gas chromatography.

    PubMed

    Zhang, Chun-Yun; Hu, Hui-Chao; Chai, Xin-Sheng; Pan, Lei; Xiao, Xian-Ming

    2013-10-04

    A novel method has been developed for the determination of adsorption partition coefficient (Kd) of minor gases in shale. The method uses samples of two different sizes (masses) of the same material, from which the partition coefficient of the gas can be determined from two independent headspace gas chromatographic (HS-GC) measurements. The equilibrium for the model gas (ethane) was achieved in 5h at 120°C. The method also involves establishing an equation based on the Kd at higher equilibrium temperature, from which the Kd at lower temperature can be calculated. Although the HS-GC method requires some time and effort, it is simpler and quicker than the isothermal adsorption method that is in widespread use today. As a result, the method is simple and practical and can be a valuable tool for shale gas-related research and applications.

  16. Albumin (BSA) Adsorption over Graphene in Aqueous Environment: Influence of Orientation, Adsorption Protocol, and Solvent Treatment.

    PubMed

    Vilhena, J G; Rubio-Pereda, Pamela; Vellosillo, Perceval; Serena, P A; Pérez, Rubén

    2016-02-23

    We report 150 ns explicit solvent MD simulations of the adsorption on graphene of albumin (BSA) in two orientations and using two different adsorption protocols, i.e., free and forced adsorption. Our results show that free adsorption occurs with little structural rearrangements. Even taking adsorption to an extreme, by forcing it with a 5 nN downward force applied during the initial 20 ns, we show that along a particular orientation BSA is able to preserve the structural properties of the majority of its binding sites. Furthermore, in all the cases considered in this work, the ibuprofen binding site has shown a strong resilience to structural changes. Finally, we compare these results with implicit solvent simulations and find that the latter predicts an extreme protein unfolding upon adsorption. The origin of this discrepancy is attributed to a poor description of the water entropic forces at interfaces in the implicit solvent methods.

  17. A novel procedure for purification of uridine 5'-monophosphate based on adsorption methodology using a hyper-cross-linked resin.

    PubMed

    Wu, Jinglan; Zhu, Hui; Liu, Yanan; Zhou, Jingwei; Zhuang, Wei; Jiao, Pengfei; Ke, Xu; Ying, Hanjie

    2015-05-01

    The conventional ion exchange process used for recovery of uridine 5'-monophosphate (UMP) from the enzymatic hydrolysate of RNA is environmentally harmful and cost intensive. In this work, an innovative benign process, which comprises adsorption technology and use of a hyper-cross-linked resin as a stationary phase is proposed. The adsorption properties of this kind of resin in terms of adsorption equilibrium as well as kinetics were evaluated. The influences of the operating conditions, i.e., initial UMP concentration, feed flow rate, and bed height on the breakthrough curves of UMP in the fixed bed system were investigated. Subsequently, a chromatographic column model was established and validated for the prediction of the experimentally attained breakthrough curves of UMP and the main impurity component (phosphate ion) with a real enzymatic hydrolysate of RNA as a feed mixture. At the end of this paper, the crystallization of UMP was carried out. The purity of the final product (uridine 5'-monophosphate disodium, UMPNa2) of over 99.5 % was obtained.

  18. Thin-Layer Chromatographic Separation of Phenols: An Undergraduate Laboratory Experiment.

    ERIC Educational Resources Information Center

    Kurth, Mark J.

    1986-01-01

    Background information, procedures used, and equipment needed are provided for an experiment in which a series of readily available, inexpensive, and relatively nontoxic phenols are separated using thin-layer chromatographic techniques. The experiment permits a discussion of how relative Rf values may be rationalized by considering a molecule's…

  19. NEAR-CONTINUOUS MEASUREMENT OF HYDROGEN SULFIDE AND CARBONYL SULFIDE BY AN AUTOMATIC GAS CHROMATOGRAPH

    EPA Science Inventory

    An automatic gas chromatograph with a flame photometric detector that samples and analyzes hydrogen sulfide and carbonyl sulfide at 30-s intervals is described. Temperature programming was used to elute trace amounts of carbon disulfide present in each injection from a Supelpak-S...

  20. 40 CFR 1065.267 - Gas chromatograph with a flame ionization detector.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Gas chromatograph with a flame ionization detector. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon...

  1. 40 CFR 1065.267 - Gas chromatograph with a flame ionization detector.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 34 2013-07-01 2013-07-01 false Gas chromatograph with a flame ionization detector. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon...

  2. 40 CFR 1065.267 - Gas chromatograph with a flame ionization detector.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 34 2012-07-01 2012-07-01 false Gas chromatograph with a flame ionization detector. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon...

  3. Chiral porous organic frameworks for asymmetric heterogeneous catalysis and gas chromatographic separation.

    PubMed

    Dong, Jinqiao; Liu, Yan; Cui, Yong

    2014-12-11

    Three chiral robust diene-based porous organic frameworks (POFs) are prepared. POF- is shown to be an efficient heterogeneous catalyst after metallation for asymmetric conjugation addition with up to 93% ee, and it can also function as a new chiral stationary phase for gas chromatographic separation of racemates.

  4. Using Aspen to Teach Chromatographic Bioprocessing: A Case Study in Weak Partitioning Chromatography for Biotechnology Applications

    ERIC Educational Resources Information Center

    Evans, Steven T.; Huang, Xinqun; Cramer, Steven M.

    2010-01-01

    The commercial simulator Aspen Chromatography was employed to study and optimize an important new industrial separation process, weak partitioning chromatography. This case study on antibody purification was implemented in a chromatographic separations course. Parametric simulations were performed to investigate the effect of operating parameters…

  5. A chromatographic survey of methods for extacting long-chain grass fructans

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Fructans were extracted under different conditions from four cool-season forages in order to develop extraction, cleanup, and chromatographic separation protocols permitting optimal analysis of long-chain fructans. Adequate sample cleanup was achieved by passage through a C18 solid-phase extractio...

  6. High-performance liquid-chromatographic separation of subcomponents of antimycin-A

    USGS Publications Warehouse

    Abidi, S.L.

    1988-01-01

    Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

  7. Liquid chromatographic assay of diatrizoic acid and its diiodo degradation products in radio-opaque solutions

    SciTech Connect

    Farag, S.A.

    1995-03-01

    A liquid chromatographic method is described for the analysis of diatrizoic acid (2,4,6-triiodo-3,5-diacetamidobenzoic acid) and its 2,4- and 2,6-diiodo degradation products in radio-opaque injection solutions. The method is accurate, precise, and linear at a concentration range of 5-50 ppm. 12 refs., 6 figs., 5 tabs.

  8. [Use of electrodialysis in the technology of desalinization of chromatographic eluates of proteins].

    PubMed

    Vasil'ev, V N; Omel'chenko, Iu N; Gusarova, E N; Iarotskiĭ, S V

    1994-05-01

    In a model of recombinant protein as an intermediate in production of rRNA-origin insulin, electrodialysis was shown to be useful in demineralization of protein chromatographic eluates. The operation conditions were developed. It was demonstrated that the electrodialysis provided higher purity of the recombinant protein.

  9. High-performance liquid chromatographic separation of subcomponents of antimycin A.

    PubMed

    Abidi, S L

    1988-08-05

    Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, A1a, A1b, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins A1, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpreted based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

  10. High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

    EPA Science Inventory

    A reverse-phase high performance liquid chromatographic (RP-HPLC) method was developed to analyze in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a RP-C16-Amide column and a ternary gradient system consistin...

  11. Adsorption characteristics of siloxanes in landfill gas by the adsorption equilibrium test

    SciTech Connect

    Nam, Sangchul; Namkoong, Wan; Kang, Jeong-Hee; Park, Jin-Kyu; Lee, Namhoon

    2013-10-15

    Highlights: • Equilibrium test was attempted to evaluate adsorption characteristics of siloxane. • L2 had higher removal efficiency in carbon compared to noncarbon adsorbents. • Total adsorption capacity of siloxane was 300 mg/g by coal activated carbon. • Adsorption characteristics rely on size of siloxane molecule and adsorbent pore. • Conversion of siloxane was caused by adsorption of noncarbon adsorbents. - Abstract: Due to the increase in energy cost by constantly high oil prices and the obligation to reduce greenhouse effect gases, landfill gas is frequently used as an alternative energy source for producing heat and electricity. Most of landfill gas utility facilities, however, are experiencing problems controlling siloxanes from landfill gas as their catalytic oxidizers are becoming fouled by silicon dioxide dust. To evaluate adsorption characteristics of siloxanes, an adsorption equilibrium test was conducted and parameters in the Freundlich and Langmuir isotherms were analyzed. Coconut activated carbon (CA1), coal activated carbon (CA2), impregnated activated carbon (CA3), silicagel (NCA1), and activated alumina (NCA2) were used for the adsorption of the mixed siloxane which contained hexamethyldisiloxane (L2), octamethylcyclotetrasiloxane (D4), and decamethylcyclopentasiloxane (D5). L2 had higher removal efficiency in noncarbon adsorbents compared to carbon adsorbents. The application of Langmuir and Freundlich adsorption isotherm demonstrated that coconut based CA1 and CA3 provided higher adsorption capacity on L2. And CA2 and NCA1 provided higher adsorption capacity on D4 and D5. Based on the experimental results, L2, D4, and D5 were converted by adsorption and desorption in noncarbon adsorbents. Adsorption affinity of siloxane is considered to be affect by the pore size distribution of the adsorbents and by the molecular size of each siloxane.

  12. Adsorption of Organic Compounds to Diesel Soot: Frontal Analysis and Polyparameter Linear Free-Energy Relationship.

    PubMed

    Lu, Zhijiang; MacFarlane, John K; Gschwend, Philip M

    2016-01-05

    Black carbons (BCs) dominate the sorption of many hydrophobic organic compounds (HOCs) in soils and sediments, thereby reducing the HOCs' mobilities and bioavailabilities. However, we do not have data for diverse HOCs' sorption to BC because it is time-consuming and labor-intensive to obtain isotherms on soot and other BCs. In this study, we developed a frontal analysis chromatographic method to investigate the adsorption of 21 organic compounds with diverse functional groups to NIST diesel soot. This method was precise and time-efficient, typically taking only a few hours to obtain an isotherm. Based on 102 soot-carbon normalized sorption coefficients (KsootC) acquired at different sorbate concentrations, a sorbate-activity-dependent polyparameter linear free-energy relationship was established: logKsootC = (3.74 ± 0.11)V + ((-0.35 ± 0.02)log ai)E + (-0.62 ± 0.10)A + (-3.35 ± 0.11)B + (-1.45 ± 0.09); (N = 102, R(2) = 0.96, SE = 0.18), where V, E, A, and B are the sorbate's McGowan's characteristic volume, excess molar refraction, and hydrogen acidity and basicity, respectively; and ai is the sorbate's aqueous activity reflecting the system's approach to saturation. The difference in dispersive interactions with the soot versus with the water was the dominant factor encouraging adsorption, and H-bonding interactions discouraged this process. Using this relationship, soot-water and sediment-water or soil-water adsorption coefficients of HOCs of interest (PAHs and PCBs) were estimated and compared with the results reported in the literature.

  13. Adsorption Isotherms and Surface Reaction Kinetics

    ERIC Educational Resources Information Center

    Lobo, L. S.; Bernardo, C. A.

    1974-01-01

    Explains an error that occurs in calculating the conditions for a maximum value of a rate expression for a bimolecular reaction. The rate expression is derived using the Langmuir adsorption isotherm to relate gas pressures and corresponding surface coverages. (GS)

  14. Capillary condensation and adsorption of binary mixtures.

    PubMed

    Weinberger, B; Darkrim-Lamari, F; Levesque, D

    2006-06-21

    The adsorption of equimolar binary mixtures of hydrogen-carbon dioxide, hydrogen-methane, and methane-carbon dioxide in porous material models is determined by grand canonical Monte Carlo simulations. The material models have an adsorbent surface similar to that of nanofibers with a herringbone structure. Our main result, which is relevant for hydrogen purification and carbon dioxide capture, is that the adsorption selectivities calculated for the mixtures can differ significantly from those deduced from simulations of the adsorption of pure gases, in particular, when one of the adsorbed gases presents a capillary condensation induced by confinement within the pore network. A comparison of our data is also made with theoretical models used in the literature for predicting the properties of the mixture adsorption.

  15. Fluorocarbon Adsorption in Hierarchical Porous Frameworks

    SciTech Connect

    Motkuri, Radha K.; Annapureddy, Harsha V.; Vijayakumar, M.; Schaef, Herbert T.; Martin, P F.; McGrail, B. Peter; Dang, Liem X.; Krishna, Rajamani; Thallapally, Praveen K.

    2014-07-09

    The adsorption behavior of a series of fluorocarbon derivatives was examined on a set of microporous metal organic framework (MOF) sorbents and another set of hierarchical mesoporous MOFs. The microporous M-DOBDC (M = Ni, Co) showed a saturation uptake capacity for R12 of over 4 mmol/g at a very low relative saturation pressure (P/Po) of 0.02. In contrast, the mesoporous MOF MIL-101 showed an exceptionally high uptake capacity reaching over 14 mmol/g at P/Po of 0.4. Adsorption affinity in terms of mass loading and isosteric heats of adsorption were found to generally correlate with the polarizability of the refrigerant with R12 > R22 > R13 > R14 > methane. These results suggest the possibility of exploiting MOFs for separation of azeotropic mixtures of fluorocarbons and use in eco-friendly fluorocarbon-based adsorption cooling and refrigeration applications.

  16. Adsorption of nisin and pediocin on nanoclays.

    PubMed

    Meira, Stela Maris Meister; Jardim, Arthur Izé; Brandelli, Adriano

    2015-12-01

    Three different nanoclays (bentonite, octadecylamine-modified montmorillonite and halloysite) were studied as potential carriers for the antimicrobial peptides nisin and pediocin. Adsorption occurred from peptide solutions in contact with nanoclays at room temperature. Higher adsorption of nisin and pediocin was obtained on bentonite. The antimicrobial activity of the resultant bacteriocin-nanoclay systems was analyzed using skimmed milk agar as food simulant and the largest inhibition zones were observed against Gram-positive bacteria for halloysite samples. Bacteriocins were intercalated into the interlayer space of montmorillonites as deduced from the increase of the basal spacing measured by X-ray diffraction (XRD) assay. Infrared spectroscopy suggested non-electrostatic interactions, such as hydrogen bonding between siloxane groups from clays and peptide molecules. Transmission electron microscopy did not show any alteration in morphologies after adsorption of antimicrobial peptides on bentonite and halloysite. These results indicate that nanoclays, especially halloysite, are suitable nanocarriers for nisin and pediocin adsorption.

  17. Ionic Adsorption and Desorption of CNT Nanoropes

    PubMed Central

    Shang, Jun-Jun; Yang, Qing-Sheng; Yan, Xiao-Hui; He, Xiao-Qiao; Liew, Kim-Meow

    2016-01-01

    A nanorope is comprised of several carbon nanotubes (CNTs) with different chiralities. A molecular dynamic model is built to investigate the ionic adsorption and desorption of the CNT nanoropes. The charge distribution on the nanorope is obtained by using a modified gradient method based on classical electrostatic theory. The electrostatic interactions among charged carbon atoms are calculated by using the Coulomb law. It was found here that the charged nanorope can adsorb heavy metal ions, and the adsorption and desorption can be realized by controlling the strength of applied electric field. The distance between the ions and the nanorope as well as the amount of ions have an effect on the adsorption capacity of the nanorope. The desorption process takes less time than that of adsorption. The study indicates that the CNT nanorope can be used as a core element of devices for sewage treatment. PMID:28335306

  18. H2O Adsorption Kinetics on Smectites

    NASA Technical Reports Server (NTRS)

    Zent, Aaron P.; Howard, J.; Quinn, R. C.

    2000-01-01

    The adsorptive equilibration of H2O with montomorillonite has been measured. At low temperatures and pressures equilibration can require many hours, effectively preventing smectites at the martian surface from responding to diurnal pressure and temperature variations.

  19. Argon adsorption and the lunar atmosphere

    NASA Technical Reports Server (NTRS)

    Bernatowicz, T. J.; Podosek, F. A.

    1991-01-01

    The results of Ar adsorption experiments on a terrestrial labradorite and lunar rock 15415 crushed in vacuo are reported. The experiments were designed to test lunar atmosphere simulation models for the behavior of Ar on the lunar surface, as determined from the Apollo 17 mass spectrometer results. These models (Hodges, 1980, 1982) used a single adsorption potential to characterize the surfaces of lunar soil grains, with the result that high (6-7 kcal/mol) heats of adsorption were inferred. The present experimental results show that very high adsorption potentials are indeed associated with fresh mineral surfaces, but that these energetic surfaces occupy only small fractions of the total surface area. Nonetheless, these small fractions of surface, if they can be maintained in the lunar regolith in steady-state condition, could be sufficient to account for the Apollo 17 mass spectrometer observations.

  20. Krypton based adsorption type cryogenic refrigerator

    NASA Technical Reports Server (NTRS)

    Jones, Jack A. (Inventor); Schember, Helene R. (Inventor)

    1989-01-01

    Krypton and a monolithic porous carbon such as Saran carbon are used respectively as the sorbate and sorbent of an adsorption type refrigerator to improve refrigeration efficiency and operational longevity.

  1. Methane Adsorption on Aggregates of Fullerenes: Site-Selective Storage Capacities and Adsorption Energies

    PubMed Central

    Kaiser, Alexander; Zöttl, Samuel; Bartl, Peter; Leidlmair, Christian; Mauracher, Andreas; Probst, Michael; Denifl, Stephan; Echt, Olof; Scheier, Paul

    2013-01-01

    Methane adsorption on positively charged aggregates of C60 is investigated by both mass spectrometry and computer simulations. Calculated adsorption energies of 118–281 meV are in the optimal range for high-density storage of natural gas. Groove sites, dimple sites, and the first complete adsorption shells are identified experimentally and confirmed by molecular dynamics simulations, using a newly developed force field for methane–methane and fullerene–methane interaction. The effects of corrugation and curvature are discussed and compared with data for adsorption on graphite, graphene, and carbon nanotubes. PMID:23744834

  2. Methane adsorption on aggregates of fullerenes: site-selective storage capacities and adsorption energies.

    PubMed

    Kaiser, Alexander; Zöttl, Samuel; Bartl, Peter; Leidlmair, Christian; Mauracher, Andreas; Probst, Michael; Denifl, Stephan; Echt, Olof; Scheier, Paul

    2013-07-01

    Methane adsorption on positively charged aggregates of C60 is investigated by both mass spectrometry and computer simulations. Calculated adsorption energies of 118-281 meV are in the optimal range for high-density storage of natural gas. Groove sites, dimple sites, and the first complete adsorption shells are identified experimentally and confirmed by molecular dynamics simulations, using a newly developed force field for methane-methane and fullerene-methane interaction. The effects of corrugation and curvature are discussed and compared with data for adsorption on graphite, graphene, and carbon nanotubes.

  3. Microcalorimetric study of adsorption and disassembling of virus-like particles on anion exchange chromatography media.

    PubMed

    Yu, Mengran; Zhang, Songping; Zhang, Yan; Yang, Yanli; Ma, Guanghui; Su, Zhiguo

    2015-04-03

    Chromatographic purification of virus-like particles (VLPs) is important to the development of modern vaccines. However, disassembly of the VLPs on the solid-liquid interface during chromatography process could be a serious problem. In this study, isothermal titration calorimetric (ITC) measurements, together with chromatography experiments, were performed on the adsorption and disassembling of multi-subunits hepatitis B virus surface antigen virus-like particles (HB-VLPs). Two gigaporous ion-exchange chromatography (IEC) media, DEAE-AP-280 nm and DEAE-POROS, were used. The application of gigaporous media with high ligand density led to significantly increased irreversible disassembling of HB-VLPs and consequently low antigen activity recovery during IEC process. To elucidate the thermodynamic mechanism of the effect of ligand density on the adsorption and conformational change of VLPs, a thermodynamic model was proposed. With this model, one can obtain the intrinsic molar enthalpy changes related to the binding of VLPs and the accompanying conformational change on the liquid-solid interface during its adsorption. This model assumes that, when intact HB-VLPs interact with the IEC media, the total adsorbed proteins contain two states, the intact formation and the disassembled formation; accordingly, the apparent adsorption enthalpy, ΔappH, which can be directly measured from ITC experiments, presents the sum of three terms: (1) the intrinsic molar enthalpy change associated to the binding of intact HB-VLPs (ΔbindHintact), (2) the intrinsic molar enthalpy change associated to the binding of HB-VLPs disassembled formation (ΔbindHdis), and (3) the enthalpy change accompanying the disassembling of HB-VLPs (ΔconfHdis). The intrinsic binding of intact HB-VLPs and the disassembled HB-VLPs to both kinds of gigaporous media (each of which has three different ligand densities), were all observed to be entropically driven as indicated by positive values of

  4. Evaluation of selectivity in homologous multimodal chromatographic systems using in silico designed antibody fragment libraries.

    PubMed

    Karkov, Hanne Sophie; Woo, James; Krogh, Berit Olsen; Ahmadian, Haleh; Cramer, Steven M

    2015-12-24

    This study describes the in silico design, surface property analyses, production and chromatographic evaluations of a diverse set of antibody Fab fragment variants. Based on previous findings, we hypothesized that the complementarity-determining regions (CDRs) constitute important binding sites for multimodal chromatographic ligands. Given that antibodies are highly diversified molecules and in particular the CDRs, we set out to examine the generality of this result. For this purpose, four different Fab fragments with different CDRs and/or framework regions of the variable domains were identified and related variants were designed in silico. The four Fab variant libraries were subsequently generated by site-directed mutagenesis and produced by recombinant expression and affinity purification to enable examination of their chromatographic retention behavior. The effects of geometric re-arrangement of the functional moieties on the multimodal resin ligands were also investigated with respect to Fab variant retention profiles by comparing two commercially available multimodal cation-exchange ligands, Capto MMC and Nuvia cPrime, and two novel multimodal ligand prototypes. Interestingly, the chromatographic data demonstrated distinct selectivity trends between the four Fab variant libraries. For three of the Fab libraries, the CDR regions appeared as major binding sites for all multimodal ligands. In contrast, the fourth Fab library displayed a distinctly different chromatographic behavior, where Nuvia cPrime and related multimodal ligand prototypes provided markedly improved selectivity over Capto MMC. Clearly, the results illustrate that the discriminating power of multimodal ligands differs between different Fab fragments. The results are promising indications that multimodal chromatography using the appropriate multimodal ligands can be employed in downstream bioprocessing for challenging selective separation of product related variants.

  5. Defluoridation of drinking water using adsorption processes.

    PubMed

    Loganathan, Paripurnanda; Vigneswaran, Saravanamuthu; Kandasamy, Jaya; Naidu, Ravi

    2013-03-15

    Excessive intake of fluoride (F), mainly through drinking water, is a serious health hazard affecting humans worldwide. There are several methods used for the defluoridation of drinking water, of which adsorption processes are generally considered attractive because of their effectiveness, convenience, ease of operation, simplicity of design, and for economic and environmental reasons. In this paper, we present a comprehensive and a critical literature review on various adsorbents used for defluoridation, their relative effectiveness, mechanisms and thermodynamics of adsorption, and suggestions are made on choice of adsorbents for various circumstances. Effects of pH, temperature, kinetics and co-existing anions on F adsorption are also reviewed. Because the adsorption is very weak in extremely low or high pHs, depending on the adsorbent, acids or alkalis are used to desorb F and regenerate the adsorbents. However, adsorption capacity generally decreases with repeated use of the regenerated adsorbent. Future research needs to explore highly efficient, low cost adsorbents that can be easily regenerated for reuse over several cycles of operations without significant loss of adsorptive capacity and which have good hydraulic conductivity to prevent filter clogging during the fixed-bed treatment process.

  6. Gibbs adsorption and the compressibility equation

    SciTech Connect

    Aranovich, G.L.; Donohue, M.D.

    1995-08-08

    A new approach for deriving the equation of state is developed. It is shown that the integral in the compressibility equation is identical to the isotherm for Gibbs adsorption in radial coordinates. The Henry, Langmuir, and Frumkin adsorption isotherms are converted into equations of state. It is shown that using Henry`s law gives an expression for the second virial coefficient that is identical to the result from statistical mechanics. Using the Langmuir isotherm leads to a new analytic expression for the hard-sphere equation of state which can be explicit in either pressure or density. The Frumkin isotherm results in a new equation of state for the square-well potential fluid. Conversely, new adsorption isotherms can be derived from equations of state using the compressibility equation. It is shown that the van der Waals equation gives an adsorption isotherm equation that describes both polymolecular adsorption and the unusual adsorption behavior observed for supercritical fluids. {copyright} {ital 1995} {ital American} {ital Institute} {ital of} {ital Physics}.

  7. Differential Heat of Adsorption and Isosteres.

    PubMed

    Tian, Yun; Wu, Jianzhong

    2017-01-31

    Heat of adsorption is a basic thermodynamic property extensively used not only for understanding thermal effects and heat management in industrial gas storage and separation processes but also for development and validation of adsorption models and materials force fields. Despite a long history of theoretical studies and a vast experimental literature, controversies often arise in the thermodynamic analysis of heat effects due to various assumptions used to describe gas adsorption and inconsistencies between direct calorimetric measurements and isosteric heat obtained from various adsorption isotherms. Here we present a rigorous theoretical procedure for predicting isosteric heat without any assumption about the geometry of porous adsorbents or operating conditions. Quantitative relations between the differential heat and various isosteres have been established with the grand-canonical Monte Carlo simulation for gas adsorption in amorphous as well as crystalline porous materials. The inconsistencies and practical issues with conventional methods for the analysis of the heat effect have been clarified in the context of the exact results for model systems. Via the resolution of a number of controversies about heat analysis, we hope that the new theoretical procedure will be adopted for both fundamental research and industrial applications of gas adsorption processes.

  8. Gas adsorption capacity of wood pellets

    DOE PAGES

    Yazdanpanah, F.; Sokhansanj, Shahabaddine; Lim, C. Jim; ...

    2016-02-03

    In this paper, temperature-programmed desorption (TPD) analysis was used to measure and analyze the adsorption of off-gases and oxygen by wood pellets during storage. Such information on how these gases interact with the material helps in the understanding of the purging/stripping behavior of off-gases to develop effective ventilation strategies for wood pellets. Steam-exploded pellets showed the lowest carbon dioxide (CO2) uptake compared to the regular and torrefied pellets. The high CO2 adsorption capacity of the torrefied pellets could be attributed to their porous structure and therefore greater available surface area. Quantifying the uptake of carbon monoxide by pellets was challengingmore » due to chemical adsorption, which formed a strong bond between the material and carbon monoxide. The estimated energy of desorption for CO (97.8 kJ/mol) was very high relative to that for CO2 (7.24 kJ/mol), demonstrating the mechanism of chemical adsorption and physical adsorption for CO and CO2, respectively. As for oxygen, the strong bonds that formed between the material and oxygen verified the existence of chemical adsorption and formation of an intermediate material.« less

  9. Gas adsorption capacity of wood pellets

    SciTech Connect

    Yazdanpanah, F.; Sokhansanj, Shahabaddine; Lim, C. Jim; Lau, A.; Bi, X. T.

    2016-02-03

    In this paper, temperature-programmed desorption (TPD) analysis was used to measure and analyze the adsorption of off-gases and oxygen by wood pellets during storage. Such information on how these gases interact with the material helps in the understanding of the purging/stripping behavior of off-gases to develop effective ventilation strategies for wood pellets. Steam-exploded pellets showed the lowest carbon dioxide (CO2) uptake compared to the regular and torrefied pellets. The high CO2 adsorption capacity of the torrefied pellets could be attributed to their porous structure and therefore greater available surface area. Quantifying the uptake of carbon monoxide by pellets was challenging due to chemical adsorption, which formed a strong bond between the material and carbon monoxide. The estimated energy of desorption for CO (97.8 kJ/mol) was very high relative to that for CO2 (7.24 kJ/mol), demonstrating the mechanism of chemical adsorption and physical adsorption for CO and CO2, respectively. As for oxygen, the strong bonds that formed between the material and oxygen verified the existence of chemical adsorption and formation of an intermediate material.

  10. Carbon dioxide adsorption in graphene sheets

    NASA Astrophysics Data System (ADS)

    Mishra, Ashish Kumar; Ramaprabhu, Sundara

    2011-09-01

    Control over the CO2 emission via automobiles and industrial exhaust in atmosphere, is one of the major concerns to render environmental friendly milieu. Adsorption can be considered to be one of the more promising methods, offering potential energy savings compared to absorbent systems. Different carbon nanostructures (activated carbon and carbon nanotubes) have attracted attention as CO2 adsorbents due to their unique surface morphology. In the present work, we have demonstrated the CO2 adsorption capacity of graphene, prepared via hydrogen induced exfoliation of graphitic oxide at moderate temperatures. The CO2 adsorption study was performed using high pressure Sieverts apparatus and capacity was calculated by gas equation using van der Waals corrections. Physical adsorption of CO2 molecules in graphene was confirmed by FTIR study. Synthesis of graphene sheets via hydrogen exfoliation is possible at large scale and lower cost and higher adsorption capacity of as prepared graphene compared to other carbon nanostructures suggests its possible use as CO2 adsorbent for industrial application. Maximum adsorption capacity of 21.6 mmole/g was observed at 11 bar pressure and room temperature (25 °C).

  11. ADSORPTION METHOD FOR SEPARATING METAL CATIONS

    DOEpatents

    Khym, J.X.

    1959-03-10

    The chromatographic separation of fission product cations is discussed. By use of this method a mixture of metal cations containing Zr, Cb, Ce, Y, Ba, and Sr may be separated from one another. Mentioned as preferred exchange adsorbents are resins containing free sulfonic acid groups. Various eluants, such as tartaric acid, HCl, and citric acid, used at various acidities, are employed to effect the selective elution and separation of the various fission product cations.

  12. Sorption characteristics and chromatographic separation of gold (I and III) from silver and base metal ions using polyurethane foams.

    PubMed

    Farag, A B; Soliman, M H; Abdel-Rasoul, O S; el-Shahawi, M S

    2007-10-10

    The influence of different parameters on the sorption profiles of trace and ultra traces of gold (I) species from the aqueous cyanide media onto the solid sorbents ion exchange polyurethane foams (IEPUFs) and commercial unloaded polyurethane foams (PUFs) based polyether type has been investigated. The retention of gold (I) species onto the investigated solid sorbents followed a first-order rate equation with an overall rate constant k in the range 2.2-2.8+/-0.2 s(-1). The sorption data of gold (I) followed Freundlich and Langmuir isotherm models. Thus, the a dual-mode of sorption mechanism involving absorption related to "weak base anion exchanger" and an added component for "surface adsorption" seems the most likely proposed dual mechanism for retention profile of gold (I) by the IEPUFs and PUFs solid sorbents. The capacity of the IEPUFs and PUFs towards gold (I) sorption calculated from the sorption isotherms was found to be 11.21+/-1.8 and 5.29+/-0.9 mg g(-1), respectively. The chromatographic separation of the spiked inorganic gold (I) from de ionized water at concentrations 5-15 microg mL(-1) onto the developed IEPUFs and PUFs packed columns at 10 mL min(-1) flow rate was successfully achieved. The retained gold (I) species were then recovered quantitatively from the IEPUFs (98.4+/-2.4%, n=5) and PUFs (95.4+/-3.4%, n=5) packed columns using perchloric acid (60 mL, 1.0 mol L(-1)) as a proper eluting agent. Thiourea (1.0 mol L(-1))-H2SO4 (0.1 mol L(-1)) system was also used as eluting agent for the recovery of gold (I) from IEPUFS (95.4+/-5.4%, n=3) and also PUFs (93.4+/-4.4%, n=3) packed columns. The performance of the IEPUFs and PUFs packed columns in terms of the height equivalent to the theoretical plates (HETP), number of plates (N), and critical and breakthrough capacities towards gold (I) species were evaluated. The developed IEPUFs packed column was applied successfully for complete retention and recovery (98.5+/-2.7) of gold (III) species spiked onto

  13. Adsorption of aqueous copper on peanut hulls

    NASA Astrophysics Data System (ADS)

    Davis, Kanika Octavia

    A method was established for measuring the adsorption of Cu(II) from aqueous solution to unmodified and modified peanut hulls at constant temperature and pH. Modification of the hulls was performed by oxidation with alkaline hydrogen peroxide. During the modification process, the hydrogen peroxide solubilizes the lignin component, making the surface more porous which increases the availability of binding sites, while simultaneously oxidizing the cellulose. The oxidation of alcohol groups creates more binding sites by creating functional groups such as COO-, which increases chelation to metal ions. Fourier transform infrared spectroscopy confirms delignification of the peanut hulls by the disappearance of carboxyl peaks of the modified hulls, which were originally produced from the lignin content. Although, oxidation is not fully confirmed, it is not ruled out because the expected carboxylate peak (1680 cm-1) maybe overshadowed by a broad peak due to OH bending of water adsorbed to the hulls. Hulls adsorbed copper from solutions in the concentration range of 50-1000 ppm of CuCl2. Concentrations of pre- and post-adsorption solutions were determined using inductively coupled plasma optical emission spectroscopy. The adsorption isotherms were fit to known two and three-parameter models, evaluated and the binding mechanism was inferred. Maximum surface coverage was 3.5 +/- 0.6 mg Cu2+ /g hull for unmodified hulls and 11 +/- 1 mg Cu2+/g hull for modified hulls. The adsorption for the hulls is best described by the Langmuir model, suggesting monolayer, homogeneous adsorption. With a free energy of adsorption of 10.5 +/- 0.9 kJ/mol for unmodified hulls and 14.5 +/-0.4 kJ/mol for modified hulls, the process is categorized as chemisorption for both types of hulls. The adsorption for both hulls is also described by the Redlich-Peterson model, giving beta nearer to 1 than 0, which further suggests homogeneous adsorption described by the Langmuir model. After rinsing the hulls

  14. Assessing the Adsorption Properties of Shales

    NASA Astrophysics Data System (ADS)

    Pini, R.

    2014-12-01

    Fine-grained rocks, such as shales, contain a significant amount of nanopores that can significantly contribute to their storage capacity through the mechanism of adsorption. The current ability to extract natural gas that is adsorbed in the rock's matrix is limited and current technology focuses primarily on the free gas in the fractures, thus leading to very low recovery efficiencies. Shales constitute also a great portion of so-called caprocks above potential CO2 sequestration sites; hereby, the adsorption process may limit the CO2 mobility within the cap-rock, thus minimizing leakage phenomena. Whether it is a reservoir or a caprock, understanding and quantifying the mechanisms of adsorption in these natural materials is key to improve the engineering design of subsurface operations. Results will be presented from a laboratory study that combines conventional techniques for the measurement of adsorption isotherms with novel methods that allows for the imaging of adsorption using x-rays. Various nanoporous materials are considered, thus including rocks, such as shales and coals, pure clay minerals and engineered adsorbents with well-defined nanopore structures, such as zeolites. Supercritical CO2 adsorption isotherms have been measured with a Rubotherm Magnetic Suspension balance by covering the pressure range 0.1-20~MPa. A medical x-ray CT scanner has been used to identify three-dimensional patterns of the adsorption properties of a packed-bed of adsorbent, thus enabling to assess the spatial variability of the adsorption isotherm. The data are analyzed by using thermodynamically rigorous measures of adsorption and a graphical method is applied for their interpretation. The density of the adsorbed phase is estimated and compared to data reported in the literature; the latter is key to disclose gas-reserves and/or potential storage capacity estimates. When evaluated against classic adsorbent materials, the adsorption mechanism in shales is further complicated by

  15. Expanded bed adsorption of human serum albumin from very dense Saccharomyces cerevesiae suspensions on fluoride-modified zirconia.

    PubMed

    Mullick, A; Flickinger, M C

    1999-11-05

    The adsorption of proteins from high cell density yeast suspensions on mixed-mode fluoride-modified zirconia (FmZr) particles (38 to 75 microm, surface area of 29 m(2)/g and density of 2.8 g/cm(3)) was investigated using human serum albumin (HSA) added to Saccharomyces cerevesiae as the model expression host. Because of the high density of the porous zirconia particles, HSA (4 mg/mL) can be adsorbed from a 100 g dry cell weight (DCW)/L yeast suspension in a threefold-expanded bed of FmZr. The expanded bed adsorption of any protein from a suspension containing >50 g DCW/L cells has not been previously reported. The FmZr bed expansion characteristics were well represented by the Richardson-Zaki correlation with a particle terminal velocity of 3.1 mm/s and a bed expansion index of 5.4. Expanded bed hydrodynamics were investigated as a function of bed expansion using residence time distribution studies with sodium nitrite as the tracer. The adsorption of HSA on FmZr exhibited features of multicomponent adsorption due to the presence of dimers. The protein binding capacity at 5% breakthrough decreased from 22 mg HSA/mL settled bed void volume for 20 g DCW/L yeast to 15 mg HSA/mL settled bed void volume for 40 g DCW/L yeast and remained unchanged for the higher yeast concentrations (60 to 100 g DCW/L). However, the batch (or equilibrium) binding capacity decreased monotonically as a function of yeast concentration (20 to 100 g DCW/L) and the binding capacity at 100 g DCW/L yeast was fivefold lower compared with that at 20 g DCW/L yeast. The lower batch binding capacity at high cell concentrations resulted from the adsorption of cells at the surface of the particles restricting access of HSA to the intraparticle surface area. Batch (or equilibrium) and column HSA adsorption results indicated that the adsorption of HSA on FmZr occurred at a time scale that may be much faster than that of yeast cells. The zirconia particles were cleaned of adsorbed HSA and yeast with a

  16. Heavy metal adsorption changes of EAF steel slag after phosphorus adsorption.

    PubMed

    Song, Guanling; Cao, Lijing; Chen, Xiao; Hou, Wenhua; Wang, Qunhui

    2012-01-01

    A kind of electric arc furnace (EAF) steel slag was phosphated, and its isothermal and dynamic adsorptions of copper, cadmium, and lead ions were measured to determine if heavy metal adsorption changes after phosphorus adsorption. The surface area increased greatly after the slag was phosphated. Isothermal adsorption experiments showed that the theoretical Q(max) of the EAF steel slag on Cu(2+), Cd(2+), and Pb(2+) improved 59, 50, and 89% respectively after it was phosphated. Dynamic adsorption results showed that the greatest adsorption capacities of unit volume of Cu(2+), Cd(2+), and Pb(2+) were 2.2, 1.8, and 1.8 times that of the column packed with original EAF steel slag when the column was packed with phosphate EAF steel slag at the same heavy metal ion concentration. The breakthrough time, the exhaustion time and elution efficiency of the column also increased when the column was packed with phosphated EAF steel slag compared with that packed with original EAF steel slag. Phosphorus adsorption could further improve the heavy metal ion adsorption of the EAF steel slag.

  17. Modeling adsorption: Investigating adsorbate and adsorbent properties

    NASA Astrophysics Data System (ADS)

    Webster, Charles Edwin

    1999-12-01

    Surface catalyzed reactions play a major role in current chemical production technology. Currently, 90% of all chemicals are produced by heterogeneously catalyzed reactions. Most of these catalyzed reactions involve adsorption, concentrating the substrate(s) (the adsorbate) on the surface of the solid (the adsorbent). Pore volumes, accessible surface areas, and the thermodynamics of adsorption are essential in the understanding of solid surface characteristics fundamental to catalyst and adsorbent screening and selection. Molecular properties such as molecular volumes and projected molecular areas are needed in order to convert moles adsorbed to surface volumes and areas. Generally, these molecular properties have been estimated from bulk properties, but many assumptions are required. As a result, different literature values are employed for these essential molecular properties. Calculated molar volumes and excluded molecular areas are determined and tabulated for a variety of molecules. Molecular dimensions of molecules are important in the understanding of molecular exclusion as well as size and shape selectivity, diffusion, and adsorbent selection. Molecular dimensions can also be used in the determination of the effective catalytic pore size of a catalyst. Adsorption isotherms, on zeolites, (crystalline mineral oxides) and amorphous solids, can be analyzed with the Multiple Equilibrium Analysis (MEA) description of adsorption. The MEA produces equilibrium constants (Ki), capacities (ni), and thermodynamic parameters (enthalpies, ΔHi, and entropies, ΔSi) of adsorption for each process. Pore volumes and accessible surface areas are calculated from the process capacities. Adsorption isotherms can also be predicted for existing and new adsorbate-adsorbent systems with the MEA. The results show that MEA has the potential of becoming a standard characterization method for microporous solids that will lead to an increased understanding of their behavior in gas

  18. Poliovirus Adsorption by 34 Minerals and Soils

    PubMed Central

    Moore, Rebecca S.; Taylor, Dene H.; Sturman, Lawrence S.; Reddy, Michael M.; Fuhs, G. Wolfgang

    1981-01-01

    The adsorption of radiolabeled infectious poliovirus type 2 by 34 well-defined soils and mineral substrates was analyzed in a synthetic freshwater medium containing 1 mM CaCl2 and 1.25 mM NaHCO3 at pH 7. In a model system, adsorption of poliovirus by Ottawa sand was rapid and reached equilibrium within 1 h at 4°C. Near saturation, the adsorption could be described by the Langmuir equation; the apparent surface saturation was 2.5 × 106 plaque-forming units of poliovirus per mg of Ottawa sand. At low surface coverage, adsorption was described by the Freundlich equation. The soils and minerals used ranged from acidic to basic and from high in organic content to organic free. The available negative surface charge on each substrate was measured by the adsorption of a cationic polyelectrolyte, polydiallyldimethylammonium chloride. Most of the substrates adsorbed more than 95% of the virus. In general, soils, in comparison with minerals, were weak adsorbents. Among the soils, muck and Genesee silt loam were the poorest adsorbents; among the minerals, montmorillonite, glauconite, and bituminous shale were the least effective. The most effective adsorbents were magnetite sand and hematite, which are predominantly oxides of iron. Correlation coefficients for substrate properties and virus adsorption revealed that the elemental composition of the adsorbents had little effect on poliovirus uptake. Substrate surface area and pH, by themselves, were not significantly correlated with poliovirus uptake. A strong negative correlation was found between poliovirus adsorption and both the contents of organic matter and the available negative surface charge on the substrates as determined by their capacities for adsorbing the cationic polyelectrolyte, polydiallyldimethylammonium chloride. PMID:6274259

  19. Toward Accurate Adsorption Energetics on Clay Surfaces

    PubMed Central

    2016-01-01

    Clay minerals are ubiquitous in nature, and the manner in which they interact with their surroundings has important industrial and environmental implications. Consequently, a molecular-level understanding of the adsorption of molecules on clay surfaces is crucial. In this regard computer simulations play an important role, yet the accuracy of widely used empirical force fields (FF) and density functional theory (DFT) exchange-correlation functionals is often unclear in adsorption systems dominated by weak interactions. Herein we present results from quantum Monte Carlo (QMC) for water and methanol adsorption on the prototypical clay kaolinite. To the best of our knowledge, this is the first time QMC has been used to investigate adsorption at a complex, natural surface such as a clay. As well as being valuable in their own right, the QMC benchmarks obtained provide reference data against which the performance of cheaper DFT methods can be tested. Indeed using various DFT exchange-correlation functionals yields a very broad range of adsorption energies, and it is unclear a priori which evaluation is better. QMC reveals that in the systems considered here it is essential to account for van der Waals (vdW) dispersion forces since this alters both the absolute and relative adsorption energies of water and methanol. We show, via FF simulations, that incorrect relative energies can lead to significant changes in the interfacial densities of water and methanol solutions at the kaolinite interface. Despite the clear improvements offered by the vdW-corrected and the vdW-inclusive functionals, absolute adsorption energies are often overestimated, suggesting that the treatment of vdW forces in DFT is not yet a solved problem. PMID:27917256

  20. A chromatographic estimate of the degree of heterogeneity of RPLC packing materials. 1. Non-endcapped polymeric C30-bonded stationary phase

    SciTech Connect

    Gritti, Fabrice; Guiochon, Georges A

    2006-01-01

    A new chromatographic method estimating the degree of heterogeneity of RPLC packing materials is based on the results of systematic measurements of the adsorption data in a wide concentration range for selected probe compounds. These data are acquired by frontal analysis (FA), modeled, and used for the calculation of the adsorption energy distribution (AED). Four compounds were used, two neutral compounds of different molecular sizes (caffeine and phenol) and two ionizable compounds of opposite charges, 2-naphthalene sulfonate, an anion, and propranololium, a cation. This work was done on a C{sub 30}-bonded silica stationary phase (Prontosil-C{sub 30}), using the same aqueous mobile phase (30% methanol, v/v) for all compounds, except that sodium chloride (25 mM) was added to elute the ionizable compounds. All four adsorption isotherms have Langmuirian behavior. The AEDs are tri-modal for phenol, quadri-modal for caffeine. The total saturation capacity of the stationary phase is four-fold lower for caffeine than for phenol, due in part to its larger molecular size. The equilibrium constants on the low-energy sites of types 1 and 2 are eight-fold larger. These two types of sites characterize the heterogeneity of the bonded layer itself. The density of the high-energy sites of types 3 and 4 is higher for caffeine, suggesting that caffeine molecules can be accommodated in some hydrophobic cages into which smaller molecules like phenol cannot. These high-energy types of sites characterize the heterogeneity of the whole stationary phase (silica support included). The ionizable compounds have larger molecules than the neutral ones and, accordingly, a lower relative density of sites of type 2 to sites of type 1. A tri-modal and a quadri-modal energy distributions were observed for the 2-naphthalene sulfonate anion and the propranololium cation, respectively. The fourth types of sites measured and its unusually high equilibrium constant are most probably due to ion

  1. Apparatus for thermal swing adsorption and thermally-enhanced pressure swing adsorption

    DOEpatents

    Wegeng, Robert S.; Rassat, Scot D.; Stenkamp, Victoria S.; TeGrotenhuis, Ward E.; Matson, Dean W.; Drost, M. Kevin; Viswanathan, Vilayanur V.

    2005-12-13

    The present invention provides compact adsorption systems that are capable of rapid temperature swings and rapid cycling. Novel methods of thermal swing adsorption and thermally-enhanced pressure swing adsorption are also described. In some aspects of the invention, a gas is passed through the adsorbent thus allowing heat exchangers to be very close to all portions of the adsorbent and utilize less space. In another aspect, the adsorption media is selectively heated, thus reducing energy costs. Methods and systems for gas adsorption/desorption having improved energy efficiency with capability of short cycle times are also described. Advantages of the invention include the ability to use (typically) 30-100 times less adsorbent compared to conventional systems.

  2. Method for thermal swing adsorption and thermally-enhanced pressure swing adsorption

    DOEpatents

    Wegeng, Robert S.; Rassat, Scot D.; Stenkamp, Victoria S.; TeGrotenhuis, Ward E.; Matson, Dean W.; Drost, M. Kevin; Viswanathan, Vilayanur V.

    2003-10-07

    The present invention provides compact adsorption systems that are capable of rapid temperature swings and rapid cycling. Novel methods of thermal swing adsorption and thermally-enhanced pressure swing adsorption are also described. In some aspects of the invention, a gas is passed through the adsorbent thus allowing heat exchangers to be very close to all portions of the adsorbent and utilize less space. In another aspect, the adsorption media is selectively heated, thus reducing energy costs. Methods and systems for gas adsorption/desorption having improved energy efficiency with capability of short cycle times are also described. Advantages of the invention include the ability to use (typically) 30-100 times less adsorbent compared to conventional systems.

  3. Method and apparatus for thermal swing adsorption and thermally-enhanced pressure swing adsorption

    DOEpatents

    Wegeng, Robert S.; Rassat, Scot D.; TeGrotenhuis, Ward E.; Drost, Kevin; Vishwanathan, Vilayanur V.

    2004-06-08

    The present invention provides compact adsorption systems that are capable of rapid temperature swings and rapid cycling. Novel methods of thermal swing adsorption and thermally-enhanced pressure swing adsorption are also described. In some aspects of the invention, a gas is passed through the adsorbent thus allowing heat exchangers to be very close to all portions of the adsorbent and utilize less space. In another aspect, the adsorption media is selectively heated, thus reducing energy costs. Methods and systems for gas adsorption/desorption having improved energy efficiency with capability of short cycle times are also described. In another aspect, the apparatus or methods utilize heat exchange channels of varying lengths that have volumes controlled to provide equal heat fluxes. Methods of fuel cell startup are also described. Advantages of the invention include the ability to use (typically) 30-100 times less adsorbent compared to conventional systems.

  4. Conceptual adsorption models and open issues pertaining to performance assessment

    SciTech Connect

    Serne, R.J.

    1991-10-01

    Recently several articles have been published that question the appropriateness of the distribution coefficient, Rd, concept to quantify radionuclide migration. Several distinct issues are raised by various critics. In this paper I provide some perspective on issues surrounding the modeling of nuclide retardation. The first section defines adsorption terminology and discusses various adsorption processes. The next section describes five commonly used adsorption conceptual models, specifically emphasizing what attributes that affect adsorption are explicitly accommodated in each model. I also review efforts to incorporate each adsorption model into performance assessment transport computer codes. The five adsorption conceptual models are (1) the constant Rd model, (2) the parametric Rd model, (3) isotherm adsorption models, (4) mass-action adsorption models, and (5) surface-complexation with electrostatics models. The final section discusses the adequacy of the distribution ratio concept, the adequacy of transport calculations that rely on constant retardation factors and the status of incorporating sophisticated adsorption models into transport codes.

  5. Adsorption of phenolic compound by aged-refuse.

    PubMed

    Xiaoli, Chai; Youcai, Zhao

    2006-09-01

    The adsorption of phenol, 2-chlorophenol, 4-chlorophenol and 2,4-dichlorophenol by aged-refuse has been studied. Adsorption isotherms have been determined for phenol, 2-chlorophenol, 4-chlorophenol and 2,4-dichlorophenol and the data fits well to the Freundlich equation. The chlorinated phenols are absorbed more strongly than the phenol and the adsorption capacity has an oblivious relationship with the numbers and the position of chlorine subsistent. The experiment data suggests that both the partition function and the chemical adsorption involve in the adsorption process. Pseudo-first-order and pseudo-second-order model were applied to investigate the kinetics of the adsorption and the results show that it fit the pseudo-second-order model. More than one step involves in the adsorption process and the overall rate of the adsorption process appears to be controlled by the chemical reaction. The thermodynamic analysis indicates that the adsorption is spontaneous and endothermic.

  6. Neptunium(V) adsorption to calcite.

    PubMed

    Heberling, Frank; Brendebach, Boris; Bosbach, Dirk

    2008-12-12

    The migration behavior of the actinyl ions U(VI)O2(2+), Np(V)O2+ and Pu(V,VI)O2(+,2+) in the geosphere is to a large extend controlled by sorption reactions (inner- or outer-sphere adsorption, ion-exchange, coprecipitation/structural incorporation) with minerals. Here NpO2+ adsorption onto calcite is studied in batch type experiments over a wide range of pH (6.0-9.4) and concentration (0.4 microM-40 microM) conditions. pH is adjusted by variation of CO2 partial pressure. Adsorption is found to be pH dependent with maximal adsorption at pH 8.3 decreasing with increasing and decreasing pH. pH dependence of adsorption decreases with increasing Np(V) concentration. EXAFS data of neptunyl adsorbed to calcite and neptunyl in the supernatant shows differences in the Np(V)-O-yl distance, 1.85+/-0.01 angstroms for the adsorbed and 1.82+/-0.01 angstroms for the solution species. The equatorial environment of the neptunyl in solution shows about 5 oxygen neighbours at 2.45+/-0.02 angstroms. For adsorbed neptunyl there are also about 5 oxygen neighbours at 2.46+/-0.01 angstroms. An additional feature in the adsorbed species' R-space spectrum can be related to carbonate neighbours, 3 to 6 carbon backscatterers (C-eq) at 3.05+/-0.03 angstroms and 3 to 6 oxygen backscatterers (O-eq2) at 3.31+/-0.02 angstroms. The differences in the Np(V)-O-yl distance and the C-eq and O-eq2 backscatterers which are only present for the adsorbed species indicate inner-sphere bonding of the adsorbed neptunyl species to the calcite surface. Experiments on adsorption kinetics indicate that after a fast surface adsorption process a continuous slow uptake occurs which may be explained by incorporation via surface dissolution and reprecipitation processes. This is also indicated by the part irreversibility of the adsorption as shown by increased KD values after desorption compared to adsorption.

  7. Phosphorus recovery using pelletized adsorptive materials ...

    EPA Pesticide Factsheets

    Phosphorous (P) is one of the essential nutrients for growth and is generally the most limiting nutrient since, it cannot be fixed from the atmosphere. Methods for recovering phosphorous from water systems already exist, but advances are being made to find a more economic, efficient, effective and easy to use method that can allow for reuse of the recovered P. One area of study is in adsorption, which involves finding the best material for adsorption of phosphorous from water and for releasing it back into the environment through desorption or leaching. The goal of this research was to first optimize the capacity for a pelletized adsorptive material that was synthesized with varying amounts of a binder material from 0-20 % and then to study recovering the phosphate for reuse. The pelletized materials were studied through kinetics experiments as well as isotherm experiments to gain insight into the adsorption capacity and mechanism. Following successful adsorption, a simple leaching study was conducted to see how much phosphate would be released back into water without any added desorption aid. Desorption was then studied by changing the pH of solution. Presenting my thesis work with a poster at ACS.

  8. Adsorption behavior of heavy metals on biomaterials.

    PubMed

    Minamisawa, Mayumi; Minamisawa, Hiroaki; Yoshida, Shoichiro; Takai, Nobuharu

    2004-09-08

    We have investigated adsorption of Cd(II) and Pb(II) at pH 2-6.7 onto the biomaterials chitosan, coffee, green tea, tea, yuzu, aloe, and Japanese coarse tea, and onto the inorganic adsorbents, activated carbon and zeolite. High adsorptive capabilities were observed for all of the biomaterials at pH 4 and 6.7. In the adsorption of Cd(II), blend coffee, tea, green tea, and coarse tea have comparable loading capacities to activated carbon and zeolite. Although activated carbon, zeolite, and chitosan are utilized in a variety of fields such as wastewater treatment, chemical and metallurgical engineering, and analytical chemistry, these adsorbents are costly. On the other hand, processing of the test biomaterials was inexpensive, and all the biomaterials except for chitosan were able to adsorb large amounts of Pb(II) and Cd(II) ions after a convenient pretreatment of washing with water followed by drying. The high adsorption capability of the biomaterials prepared from plant materials is promising in the development of a novel, low-cost adsorbent. From these results, it is concluded that heavy metal removal using biomaterials would be an effective method for the economic treatment of wastewater. The proposed adsorption method was applied to the determination of amounts of Cd(II) and Pb(II) in water samples.

  9. Sulfate adsorption in Michigan forest soils

    SciTech Connect

    MacDonald, N.W.

    1987-01-01

    The occurrence of acidic atmospheric deposition raised concerns over adverse cation leaching effects on Michigan forest soils with low cation exchange capacities. Leaching effects of acid deposition depend on mobility of sulfate in the soil. Little was known, however, concerning the ability of these soils to adsorb sulfate. The objectives of this study were to determine the ability of representative Michigan forest soils to adsorb sulfate, to relate sulfate adsorption to soil properties, and to develop equations to predict sulfate adsorption in similar forest soils. Frigid zone soil series studied were Grayling (Typic Udipsamments), Rubicon (Entic Haplorthods), Kalkaska (Typic Haplorthods), and Montcalm (Eutric Glossoboralfs). Mesic zone series studied were Spinks (Psammentic Hapludals) and Oshtemo (Typic Hapludalfs). Six randomly located pedons of each series were sampled. Sulfate adsorption was determined by shaking 10 gram soil samples for 24 hours in 50 mL 0.01 M CaCl/sub 2/ solution containing 10 mg SO/sub 4/-S L/sup -1/. Solution filtrates were turbidimetrically analyzed for SO/sub 4/-S and adsorption was calculated from reduction in SO/sub 4/-S concentration. Bw, Bs, and Bh horizons of frigid zone soils and E and Bt horizons of mesic zone soils had the highest sulfate adsorbing abilities. No significant differences were found between series in total sulfate adsorptive capacity.

  10. DNA adsorption by indium tin oxide nanoparticles.

    PubMed

    Liu, Biwu; Liu, Juewen

    2015-01-01

    The high conductivity and optical transparency of indium tin oxide (ITO) has made it a popular material in the electronic industry. Recently, its application in biosensors is also explored. To understand its biointerface chemistry, we herein investigate its interaction with fluorescently labeled single-stranded oligonucleotides using ITO nanoparticles (NPs). The fluorescence of DNA is efficiently quenched after adsorption, and the interaction between DNA and ITO NPs is strongly dependent on the surface charge of ITO. At low pH, the ITO surface is positively charged to afford a high DNA adsorption capacity. Adsorption is also influenced by the sequence and length of DNA. For its components, In2O3 adsorbs DNA more strongly while SnO2 repels DNA at neutral pH. The DNA adsorption property of ITO is an averaging result from both components. DNA adsorption is confirmed to be mainly by the phosphate backbone via displacement experiments using free phosphate or DNA bases. Last, DNA-induced DNA desorption by forming duplex DNA is demonstrated on ITO, while the same reaction is more difficult to achieve on other metal oxides including CeO2, TiO2, and Fe3O4 because these particles adsorb DNA more tightly.

  11. Adsorption of Wine Constituents on Functionalized Surfaces.

    PubMed

    Mierczynska-Vasilev, Agnieszka; Smith, Paul A

    2016-10-18

    The adsorption of macromolecules on solid surfaces is of great importance in the field of nanotechnology, biomaterials, biotechnological, and food processes. In the field of oenology adsorption of wine macromolecules such as polyphenols, polysaccharides, and proteins is much less desirable on membrane materials because of fouling and reduced filtering performance. On the other hand, adsorption of these molecules on processing aids is very beneficial for achieving wine clarity and stability. In this article, the effect of surface chemical functionalities on the adsorption of white, rosé, and red wine constituents was evaluated. Allylamine, acrylic acid, and ethanol were selected as precursors for plasma polymerization in order to generate coatings rich in amine, carboxyl, and hydroxyl chemical groups, respectively. The surface chemical functionalities were characterized by X-ray photoelectron spectroscopy (XPS) and the ability of different surface chemical functionalities to adsorb wine constituents were characterized by quartz crystal microbalance with dissipation (QCM-D) and atomic force microscopy (AFM). The results demonstrated that the amine and carboxyl modified surfaces encourage adsorption of constituents from white wine. The hydroxyl modified surfaces have the ability to preferentially adsorb rosé wine constituents, whereas red wine adsorbed to the highest extent on acrylic acid surface.

  12. Adsorption of phenanthrene on natural snow.

    PubMed

    Domine, Florent; Cincinelli, Alessandra; Bonnaud, Elodie; Martellini, Tania; Picaud, Sylvain

    2007-09-01

    The snowpack is a reservoir for semivolatile organic compounds (SVOCs) and, in particular, for persistent organic pollutants (POPs), which are sequestered in winter and released to the atmosphere or hydrosphere in the spring. Modeling these processes usually assumes that SVOCs are incorporated into the snowpack by adsorption to snow surfaces, but this has never been proven because the specific surface area (SSA) of snow has never been measured together with snow composition. Here we expose natural snow to phenanthrene vapors (one of the more volatile POPs) and measure for the first time both the SSA and the chemical composition of the snow. The results are consistent with an adsorption equilibrium. The measured Henry's law constant is H(Phen)(T) = 2.88 x 10(22) exp(-10660/7) Pa m2 mol(-1), with Tin Kelvin. The adsorption enthalpy is delta H(ads) = -89 +/- 18 kJ mol(-1). We also perform molecular dynamics calculations of phenanthrene adsorption to ice and obtain AHads = -85 +/- 8 kJ mol(-1), close to the experimental value. Results are applied to the adsorption of phenanthrene to the Arctic and subarctic snowpacks. The subarctic snowpack, with a low snow area index (SAI = 1000), is a negligible reservoir of phenanthrene, butthe colder Arctic snowpack, with SAI = 2500, sequesters most of the phenanthrene present in the (snow + boundary layer) system.

  13. Adsorption of gases on carbon molecular sieves

    SciTech Connect

    Vyas, S.N.; Patwardhan, S.R.; Vijayalakshmi, S. . Dept. of Chemical Engineering); Ganesh, K.S. )

    1994-12-01

    Adsorption on carbon molecular sieves (CMS) prepared by coke deposition has become an interesting area of adsorption due to its microporous nature and favorable separation factor on size and shape selectivity basis for many gaseous systems. In the present work CMS was synthesized from coconut shell through three major steps, namely, carbonization, activation, and coke deposition by hydrocarbon cracking. The crushed, washed, and sieved granules of coconut shell (particle size 2--3 mm) were pretreated with sodium silicate solution and oven-dried at 150 C to create the inorganic sites necessary for coke deposition. Carbonization and activation of the dried granules were carried out at 800 C, for 30 min each. The activated char thus produced was subjected to hydrocarbon cracking at 600 C for periods varying from 30 to 180 min. The product samples were characterized in terms of adsorption isotherm, kinetic adsorption curve, surface area, pore volume, pore size distribution, and characteristic energy for adsorption by using O[sub 2], N[sub 2], C[sub 2]H[sub 2], CO[sub 2], C[sub 3]H[sub 6], and CH[sub 4].

  14. Comparative isosteric ion adsorption for minerals

    NASA Technical Reports Server (NTRS)

    Omenyi, Samuel N.; Herren, Blair J.; Snyder, Robert S.; Seaman, Geoffrey V. F.

    1986-01-01

    A comparative isosteric ion adsorption study for minerals (kaolinite, rutile, and quartz) was performed in aqueous solutions of CaCl2, LaCl3, and Th(NO3)4 in the presence of the neutral salt NaCl. It was observed that the concentration of Ca(2+) ions required to produce a standard reduction in the electrophoretic mobility of mineral particles was always appreciably greater than the concentration required for the Th(4+) ions. The effectiveness of adsorption of the cations differed from particle to particle and showed that ion adsorption on a mineral surface depends, among other things, on the nature of the mineral surface and on the particular adsorbed cation. The number of cation binding sites on mineral surfaces and the electrochemical free energies of cation adsorption were calculated. It was found that the adsorption energy of La(3+) and Th(4+) ions on rutile, kaolinite, and quartz was greater than that of Ca(2+) on these minerals.

  15. Chromatographic separation of three monoclonal antibody variants using multicolumn countercurrent solvent gradient purification (MCSGP).

    PubMed

    Müller-Späth, Thomas; Aumann, Lars; Melter, Lena; Ströhlein, Guido; Morbidelli, Massimo

    2008-08-15

    Multicolumn countercurrent solvent gradient purification (MCSGP) is a continuous chromatographic process developed in recent years (Aumann and Morbidelli, 2007a; Aumann et al., 2007) that is particularly suited for applications in the field of bioseparations. Like batch chromatography, MCSGP is suitable for three-fraction chromatographic separations and able to perform solvent gradients but it is superior in terms of solvent consumption, yield, purity, and productivity due to the countercurrent movement of the liquid and the solid phases. In this work, the MCSGP process is applied to the separation of three monoclonal antibody variants on a conventional preparative cation exchange resin. The experimental process performance was compared to simulations based on a lumped kinetic model. Yield and purity values of the target variant of 93%, respectively were obtained experimentally. The batch reference process was clearly outperformed by the MCSGP process.

  16. Gas chromatographic-mass spectrometric analysis of volatile amines produced by several strains of Clostridium.

    PubMed

    Pons, J L; Rimbault, A; Darbord, J C; Leluan, G

    1985-02-08

    A gas chromatographic--mass spectrometric technique is proposed for the analysis of volatile amines which were isolated from Clostridium cultures by vacuum distillation and concentrated as hydrochloride salts. Headspace sampling after alkalinization of the salts under vacuum was the most suitable for subsequent gas chromatographic analysis. With ammonia-loaded helium as carrier gas, methylamines were separated on 4.8% PEG 2OM + 0.3% potassium hydroxide on Carbopack B, and other volatile amines on 28% Pennwalt 223 + 4% potassium hydroxide on Gas-Chrom R. Bacterial volatile amines (dimethylamine, trimethylamine, isobutylamine, 3-methylbutylamine, etc.) were detected with a flame-ionization detector and identified by gas chromatography--mass spectrometry in electron-impact and chemical ionization modes.

  17. Development of gas chromatographic system for dissolved organic carbon analysis in seawater

    SciTech Connect

    Chipman, D.W.; Takahashi, T.

    1992-12-01

    During the first six months of this two-year grant, we have completed the construction of the analytical portion of a prototype gas chromatograph-based system for the analysis of dissolved organic carbon in seawater. We also have begun testing the procedures to be used to cryogenically concentrate and transfer carbon dioxide from the oxidizing atmosphere of the high-temperature furnace into the reducing hydrogen carrier gas of the gas chromatograph. During the second half of the first year, we will construct the high-temperature catalytic oxidation furnace and test the entire system on laboratory-prepared aqueous solutions of various organic compounds. Also during this period, we will take part in an initial scoping study within the Cape Hatteras field area on board the R/V Gyre. This study will involve both the collection of samples of seawater for organic and inorganic carbon analysis and the measurement of surface-water pCO[sub 2].

  18. Development of gas chromatographic system for dissolved organic carbon analysis in seawater. Annual progress report

    SciTech Connect

    Chipman, D.W.; Takahashi, T.

    1992-12-01

    During the first six months of this two-year grant, we have completed the construction of the analytical portion of a prototype gas chromatograph-based system for the analysis of dissolved organic carbon in seawater. We also have begun testing the procedures to be used to cryogenically concentrate and transfer carbon dioxide from the oxidizing atmosphere of the high-temperature furnace into the reducing hydrogen carrier gas of the gas chromatograph. During the second half of the first year, we will construct the high-temperature catalytic oxidation furnace and test the entire system on laboratory-prepared aqueous solutions of various organic compounds. Also during this period, we will take part in an initial scoping study within the Cape Hatteras field area on board the R/V Gyre. This study will involve both the collection of samples of seawater for organic and inorganic carbon analysis and the measurement of surface-water pCO{sub 2}.

  19. A novel chromatographic method allows on-line reanalysis of the proteome.

    PubMed

    Waanders, Leonie F; Almeida, Reinaldo; Prosser, Simon; Cox, Jürgen; Eikel, Daniel; Allen, Mark H; Schultz, Gary A; Mann, Matthias

    2008-08-01

    Liquid chromatography combined with electrospray ionization is widely used for direct analysis of polar and labile molecules by LCMS. The on-line coupling in LCMS is a major strength but also causes a principal limitation that each eluting analyte has to be analyzed immediately and is not available for detailed interrogation after the LCMS run. Here we developed a new chromatographic strategy, which removes this limitation. After column separation the flow is split, one portion is analyzed directly, and the other is diverted to a capture capillary. After the direct LCMS run, the flow is switched, and the portion stored in the capillary is analyzed ("replay run"). We describe a setup consisting of an analytical column, a splitting valve, and a focusing column, which performs at full sensitivity and undiminished chromatographic resolution. We demonstrate three principal advantages of this system: nearly continuous MS utilization, duplicate analysis without requirement for additional sample, and targeting of important but undersampled features in the replay run.

  20. Chromatographic separation as selection process for prebiotic evolution and the origin of the genetic code.

    PubMed

    Lehmann, U

    1985-01-01

    A model for the evolution of a translation apparatus has been suggested where oligonucleotides in a hairpin conformation act as primordial adapters. Specifically activated amino acids are assumed to be attached to these hairpin molecules. For the specific activation, a chromatographic separation of, e.g. ala and CMP from gly and GMP can be accomplished on silica (e.g. of volcanic origin) with aqueous salt solutions. Other adsorbents like clays (kaolin, bentonite, montmorillonite), different silicates (florisil, magnesium trisilicate, calcium silicate, talc), hydroxyapatite, barium sulfate, calcium carbonate, calcium fluoride and titanoxide have been examined as model systems for the separation of nucleotides, nucleosides and amino acids on mineral surfaces. The possible role of chromatographic separation of amino acids for the formation of proteinoids, composed of selected amino acids, is also considered.

  1. Chromatographic separation of germanium and arsenic for the production of high purity (77)As.

    PubMed

    Gott, Matthew D; DeGraffenreid, Anthony J; Feng, Yutian; Phipps, Michael D; Wycoff, Donald E; Embree, Mary F; Cutler, Cathy S; Ketring, Alan R; Jurisson, Silvia S

    2016-04-08

    A simple column chromatographic method was developed to isolate (77)As (94±6% (EtOH/HCl); 74±11 (MeOH)) from germanium for potential use in radioimmunotherapy. The separation of arsenic from germanium was based on their relative affinities for different chromatographic materials in aqueous and organic environments. Using an organic or mixed mobile phase, germanium was selectively retained on a silica gel column as germanate, while arsenic was eluted from the column as arsenate. Subsequently, enriched (76)Ge (98±2) was recovered for reuse by elution with aqueous solution (neutral to basic). Greater than 98% radiolabeling yield of a (77)As-trithiol was observed from methanol separated [(77)As]arsenate [17].

  2. Systematic toxicological analysis of drugs and poisons in biosamples by hyphenated chromatographic and spectroscopic techniques.

    PubMed

    Polettini, A

    1999-10-15

    The introduction of hyphenated chromatographic-spectroscopic techniques represented a substantial step-forward for Systematic Toxicological Analysis (STA), increasing the amount and quality of information obtainable from the analysis of a biological sample, and enhancing the possibilities of identifying unknown drugs and poisons. STA methods based either on GC-MS or on HPLC-UV published in the last decade are reviewed in this paper. The different analytical phases, i.e. sample preparation (pretreatment, extraction, derivatisation), chromatographic separation and detection/identification are examined in detail in order to emphasise the complementarity of the two approaches. In addition, the first STA method based on HPLC-MS is illustrated and some applications of TLC-UV to drug screening are also described. Finally, an overview of semi- and fully-automated STA methods is given.

  3. Chromatographic retention-activity relationships for prediction of the toxicity pH-dependence of phenols.

    PubMed

    Bermúdez-Saldaña, J M; Escuder-Gilabert, L; Medina-Hernández, M J; Villanueva-Camañas, R M; Sagrado, S

    2007-08-01

    An investigation of the use of the chromatographic retention (log k) as an in vitro approach for modeling the pH-dependence of the toxicity to Guppy of phenols is developed. A data set of 19 phenols with available experimental toxicity-pH data was used. The importance of the mechanism of toxic action (MOA) of phenols was studied. log k data at three pH values were used for the phenols classification and two groups or 'MODEs' were identified. For one 'MODE' a quantitative retention-activity relationship (QRAR) model was calculated. Finally, the model was used to assess the toxicity to Guppy of phenols at different pH values. The results of this investigation suggest that chromatographic retention data allows fish toxicity modeling, in the 5.5-8 pH range of interest.

  4. Chromatographic multivariate quality control of pharmaceuticals giving strongly overlapped peaks based on the chromatogram profile.

    PubMed

    Escuder-Gilabert, L; Ruiz-Roch, D; Villanueva-Camañas, R M; Medina-Hernández, M J; Sagrado, S

    2004-03-12

    In the present paper, the simultaneous quantification of two analytes showing strongly overlapped chromatographic peaks (alpha = 1.02), under the assumption that both available equipment and training of the laboratory staff are basic, is studied. A pharmaceutical preparation (Mutabase) containing two drugs of similar physicochemical properties (amitriptyline and perphenazine) is selected as case of study. The assays are carried out under realistic working conditions (i.e. routine testing laboratories). Uncertainty considerations are introduced in the study. A partial least squares model is directly applied to the chromatographic data (with no previous signal transformation) to perform quality control of the pharmaceutical formulation. Under the adequate protocol, the relative error in prediction of analytes is within the tolerances found in the pharmacopeia (10%). For spiked samples simulating formulation mistakes, the errors found have the same magnitude and sign to those provoked.

  5. Highly sensitive gas chromatographic determination of ethanol in human urine samples.

    PubMed

    Zilly, Michael; Langmann, Peter; Lenker, Ulrike; Satzinger, Verena; Schirmer, Diana; Klinker, Hartwig

    2003-12-25

    In order to evaluate recent alcohol consumption, a very sensitive and specific gas chromatographic method for ethanol determination in human urine samples was developed. The non-invasive method was performed without any pretreatment and carried out on a Stabilwax capillary column, 30 m x 0.53 mm x 1.0 microm film thickness. Helium was used as carrier gas with a constant inlet pressure of 27.72 kPa (0.277 bar) and a flame ionization detector (FID). Quantification was performed with the use of acetonitrile as an internal standard (IS). The calibration curve was linear throughout the concentration range from 0.5 to 500 mg/l. The calculated intra- and inter-day coefficients of variation were below 8%. A clear chromatographic separation of ethanol from methanol, acetone, 1-propanol and 2-propanol was achieved.

  6. A review of the extraction and chromatographic determination methods for the analysis of parabens.

    PubMed

    Piao, Chunying; Chen, Ligang; Wang, Yu

    2014-10-15

    Parabens are a family of most widely used antimicrobial preservatives in food ingredients, cosmetic consumer products and pharmaceutical preparations. But several recent studies have cautioned that exposure to parabens may have more harmful consequences on animal and human health than what we realized previously, which made the analysis of parabens necessary. In this paper, we reviewed main sample preparation methods and chromatographic analysis methods proposed in formerly published works dealing with the analysis of parabens in different matrices. The sample preparation methods included ultrasonic assisted extraction, supercritical fluid extraction, pressurized liquid extraction, solid phase extraction, solid phase microextraction, liquid phase microextraction, dispersive liquid-liquid microextraction, stir bar sorptive extraction and matrix solid phase dispersion. The chromatographic analysis methods involved liquid chromatography, gas chromatography, and capillary electrophoresis.

  7. Superheated water as chromatographic eluent for parabens separation on octadecyl coated zirconia stationary phase.

    PubMed

    Dugo, Paola; Buonasera, Katia; Crupi, Maria Lucia; Cacciola, Francesco; Dugo, Giovanni; Mondello, Luigi

    2007-05-01

    In this study, the use of pure water at superheated temperatures, between 100 and 200 degrees C, as a mobile phase for RP separation is explored. Instrumental parameters, such as temperature, flow rate, preheating and cooling, have shown significant effects on the quality of the chromatographic peaks. The properties of superheated water as an eluent were investigated by observing the chromatographic behaviour of four parabens on a carbon-clad zirconia (ZR) phase with covalently bonded octadecyl groups. Results were compared with those obtained at 30 degrees C on a silica-based phase with octadecyl groups, using water and ACN as mobile phase. The optimized method was finally applied to analyse parabens in a commercial body cream.

  8. A novel thermodynamic state recursion method for description of nonideal nonlinear chromatographic process of frontal analysis.

    PubMed

    Liu, Qian; OuYang, Liangfei; Liang, Heng; Li, Nan; Geng, Xindu

    2012-06-01

    A novel thermodynamic state recursion (TSR) method, which is based on nonequilibrium thermodynamic path described by the Lagrangian-Eulerian representation, is presented to simulate the whole chromatographic process of frontal analysis using the spatial distribution of solute bands in time series like as a series of images. TSR differs from the current numerical methods using the partial differential equations in Eulerian representation. The novel method is used to simulate the nonideal, nonlinear hydrophobic interaction chromatography (HIC) processes of lysozyme and myoglobin under the discrete complex boundary conditions. The results show that the simulated breakthrough curves agree well with the experimental ones. The apparent diffusion coefficient and the Langmuir isotherm parameters of the two proteins in HIC are obtained by the state recursion inverse method. Due to its the time domain and Markov characteristics, TSR is applicable to the design and online control of the nonlinear multicolumn chromatographic systems.

  9. Liquid chromatographic determination of benzo(a)pyrene in total particulate matter of cigarette smoke

    SciTech Connect

    Tomkins, B.A.; Jenkins, R.A.; Griest, W.H.; Reagan, R.R.; Holladay, S.K.

    1985-09-01

    The benzo(a)pyrene (BaP) delivery of reference and commercially available tobacco cigarettes, as well as reference and placebo marijuana cigarettes, is determined using a sequential liquid chromatographic/liquid chromatographic procedure. The total particulate matter of sample cigarette smoke is collected using a Cambridge filter pad, which is ultrasonically extracted with acetone. The resulting extract is filtered, then fractionated using semipreparative-scale normal phase liquid chromatography (LC). Quantitative determination is achieved using analytical-scale reverse phase LC equipped with a fluorescence detector. The method is precise (+/- 10-15% relative standard deviation) and yields 85% or better BaP recovery at the ng/cig. level. A single pad may be analyzed in 8 person-hours, while a more typical lot of 12 pads (6 pads each for 2 cigarette brands) may be analyzed in 10 person-days.

  10. Chromatographic fingerprint analysis of yohimbe bark and related dietary supplements using UHPLC/UV/MS.

    PubMed

    Sun, Jianghao; Chen, Pei

    2012-03-05

    A practical ultra high-performance liquid chromatography (UHPLC) method was developed for fingerprint analysis of and determination of yohimbine in yohimbe barks and related dietary supplements. Good separation was achieved using a Waters Acquity BEH C(18) column with gradient elution using 0.1% (v/v) aqueous ammonium hydroxide and 0.1% ammonium hydroxide in methanol as the mobile phases. The study is the first reported chromatographic method that separates corynanthine from yohimbine in yohimbe bark extract. The chromatographic fingerprint analysis was applied to the analysis of 18 yohimbe commercial dietary supplement samples. Quantitation of yohimbine, the traditional method for analysis of yohimbe barks, were also performed to evaluate the results of the fingerprint analysis. Wide variability was observed in fingerprints and yohimbine content among yohimbe dietary supplement samples. For most of the dietary supplements, the yohimbine content was not consistent with the label claims.

  11. Gas chromatographic analysis of polyhydroxybutyrate in activated sludge: a round-robin test.

    PubMed

    Baetens, D; Aurola, A M; Foglia, A; Dionisi, D; van Loosdrecht, M C M

    2002-01-01

    Polyhydroxyalkanoates (PHA) and poly-beta-hydroxybutyrate (PHB) in particular have become compounds which is routinely investigated in wastewater research. The PHB analysis method has only recently been applied to activated sludge samples where PHA contents might be relatively low. This urges the need to investigate the reproducibility of the gas chromatographic method for PHB analysis. This was evaluated in a round-robin test in 5 European laboratories with samples from lab-scale and full-scale enhanced biological phosphorus removal systems. It was shown that the standard deviation of measurements in each lab and the reproducibility between the labs was very good. Experimental results obtained by different laboratories using this analysis method can be compared. Sludge samples with PHB contents varying between 0.3 and 22.5 mg PHB/mg sludge were analysed. The gas chromatographic method allows for PHV, PH2MB and PH2MV analysis as well.

  12. Estimation of the vapor pressure of petroleum distillate fractions from gas chromatographic data

    SciTech Connect

    Eggertsen, F.T.; Nygard, N.R.; Nickoley, L.D.

    1980-11-01

    The vapor pressure of petroleum distillate fractions is estimated conveniently by applying ideal gas and solution laws to gas chromatographic data. The vapor pressure is computed as a summation of the partial pressures for carbon number groups in the chromatogram, each partial pressure being derived as the product of mole fraction, determined from the chromatogram, and saturation pressure, calculated using the Antoine equation. A rapid method of computation with a programmable calculator was used. The method assumes approximate conformance to Raoult's and Dalton's laws relating to partial pressures from a solution. The results generally agree well with values obtained manometrically. Advantages of the method are the general availability of suitable gas chromatographic equipment, convenience and speed of the procedure and calculations, applicability over a wide range of volatility, freedom from temperature equilibration problems, and small sample requirement. 4 figures, 6 tables.

  13. Adsorption of plutonium oxide nanoparticles.

    PubMed

    Schmidt, Moritz; Wilson, Richard E; Lee, Sang Soo; Soderholm, L; Fenter, P

    2012-02-07

    Adsorption of monodisperse cubic plutonium oxide nanoparticles ("Pu-NP", [Pu(38)O(56)Cl(x)(H(2)O)(y)]((40-x)+), with a fluorite-related lattice, approximately 1 nm in edge size) to the muscovite (001) basal plane from aqueous solutions was observed in situ (in 100 mM NaCl background electrolyte at pH 2.6). Uptake capacity of the surface quantified by α-spectrometry was 0.92 μg Pu/cm(2), corresponding to 10.8 Pu per unit cell area (A(UC)). This amount is significantly larger than that of Pu(4+) needed for satisfying the negative surface charge (0.25 Pu(4+) for 1 e(-)/A(UC)). The adsorbed Pu-NPs cover 17% of the surface area, determined by X-ray reflectivity (XR). This correlates to one Pu-NP for every 14 unit cells of muscovite, suggesting that each particle compensates the charge of the unit cells onto which it adsorbs as well as those in its direct proximity. Structural investigation by resonant anomalous X-ray reflectivity distinguished two different sorption states of Pu-NPs on the surface at two different regimes of distance from the surface. A fraction of Pu is distributed within 11 Å from the surface. The distribution width matches the Pu-NP size, indicating that this species represents Pu-NPs adsorbed directly on the surface. Beyond the first layer, an additional fraction of sorbed Pu was observed to extend more broadly up to more than 100 Å from the surface. This distribution is interpreted as resulting from "stacking" or aggregation of the nanoparticles driven by sorption and accumulation of Pu-NPs at the interface although these Pu-NPs do not aggregate in the solution. These results are the first in situ observation of the interaction of nanoparticles with a charged mineral-water interface yielding information important to understanding the environmental transport of Pu and other nanophase inorganic species.

  14. How Much Can We Learn from a Single Chromatographic Experiment? A Bayesian Perspective.

    PubMed

    Wiczling, Paweł; Kaliszan, Roman

    2016-01-05

    In this work, we proposed and investigated a Bayesian inference procedure to find the desired chromatographic conditions based on known analyte properties (lipophilicity, pKa, and polar surface area) using one preliminary experiment. A previously developed nonlinear mixed effect model was used to specify the prior information about a new analyte with known physicochemical properties. Further, the prior (no preliminary data) and posterior predictive distribution (prior + one experiment) were determined sequentially to search towards the desired separation. The following isocratic high-performance reversed-phase liquid chromatographic conditions were sought: (1) retention time of a single analyte within the range of 4-6 min and (2) baseline separation of two analytes with retention times within the range of 4-10 min. The empirical posterior Bayesian distribution of parameters was estimated using the "slice sampling" Markov Chain Monte Carlo (MCMC) algorithm implemented in Matlab. The simulations with artificial analytes and experimental data of ketoprofen and papaverine were used to test the proposed methodology. The simulation experiment showed that for a single and two randomly selected analytes, there is 97% and 74% probability of obtaining a successful chromatogram using none or one preliminary experiment. The desired separation for ketoprofen and papaverine was established based on a single experiment. It was confirmed that the search for a desired separation rarely requires a large number of chromatographic analyses at least for a simple optimization problem. The proposed Bayesian-based optimization scheme is a powerful method of finding a desired chromatographic separation based on a small number of preliminary experiments.

  15. Similarity analyses of chromatographic fingerprints as tools for identification and quality control of green tea.

    PubMed

    Alaerts, G; Van Erps, J; Pieters, S; Dumarey, M; van Nederkassel, A M; Goodarzi, M; Smeyers-Verbeke, J; Vander Heyden, Y

    2012-12-01

    Similarity assessment of complex chromatographic profiles of herbal medicinal products is important as a potential tool for their identification. Mathematical similarity parameters have the advantage to be more reliable than visual similarity evaluations of often subtle differences between the fingerprint profiles. In this paper, different similarity analysis (SA) parameters are applied on green-tea chromatographic fingerprint profiles in order to test their ability to identify (dis)similar tea samples. These parameters are either based on correlation or distance measurements. They are visualised in colour maps and evaluation plots. Correlation (r) and congruence (c) coefficients are shown to provide the same information about the similarity of samples. The standardised Euclidean distance (ds) reveals less information than the Euclidean distance (de), while Mahalanobis distances (dm) are unsuitable for the similarity assessment of chromatographic fingerprints. The adapted similarity score (ss*) combines the advantages of r (or c) and de. Similarity analysis based on correlation is useful if concentration differences between samples are not important, whereas SA based on distances also detects concentration differences well. The evaluation plots including statistical confidence limits for the plotted parameter are found suitable for the evaluation of new suspected samples during quality assurance. The ss* colour maps and evaluation plots are found to be the best tools (in comparison to the other studied parameters) for the distinction between deviating and genuine fingerprints. For all studied data sets it is confirmed that adequate data pre-treatment, such as aligning the chromatograms, prior to the similarity assessment, is essential. Furthermore, green-tea samples chromatographed on two dissimilar High-Performance Liquid Chromatography (HPLC) columns provided the same similarity assessment. Combining these complementary fingerprints did not improve the similarity

  16. Evaluation of the suitability of chromatographic systems to predict human skin permeation of neutral compounds.

    PubMed

    Hidalgo-Rodríguez, Marta; Soriano-Meseguer, Sara; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

    2013-12-18

    Several chromatographic systems (three systems of high-performance liquid chromatography and two micellar electrokinetic chromatography systems) besides the reference octanol-water partition system are evaluated by a systematic procedure previously proposed in order to know their ability to model human skin permeation. The precision achieved when skin-water permeability coefficients are correlated against chromatographic retention factors is predicted within the framework of the solvation parameter model. It consists in estimating the contribution of error due to the biological and chromatographic data, as well as the error coming from the dissimilarity between the human skin permeation and the chromatographic systems. Both predictions and experimental tests show that all correlations are greatly affected by the considerable uncertainty of the skin permeability data and the error associated to the dissimilarity between the systems. Correlations with much better predictive abilities are achieved when the volume of the solute is used as additional variable, which illustrates the main roles of both lipophilicity and size of the solute to penetrate through the skin. In this way, the considered systems are able to give precise estimations of human skin permeability coefficients. In particular, the HPLC systems with common C18 columns provide the best performances in emulating the permeation of neutral compounds from aqueous solution through the human skin. As a result, a methodology based on easy, fast, and economical HPLC measurements in a common C18 column has been developed. After a validation based on training and test sets, the method has been applied with good results to the estimation of skin permeation of several hormones and pesticides.

  17. Chromatographic fingerprinting: An innovative approach for food 'identitation' and food authentication - A tutorial.

    PubMed

    Cuadros-Rodríguez, Luis; Ruiz-Samblás, Cristina; Valverde-Som, Lucia; Pérez-Castaño, Estefanía; González-Casado, Antonio

    2016-02-25

    Fingerprinting methods describe a variety of analytical methods that provide analytical signals related to the composition of foodstuffs in a non-selective way such as by collecting a spectrum or a chromatogram. Mathematical processing of the information in such fingerprints may allow the characterisation and/or authentication of foodstuffs. In this context, the particular meaning of 'fingerprinting', in conjunction with 'profiling', is different from the original meanings used in metabolomics. This fact has produced some confusion with the use of these terms in analytical papers. Researchers coming from the metabolomic field could use 'profiling' or 'fingerprinting' on a different way to researchers who are devoted to food science. The arrival of an eclectic discipline, named 'foodomics' has not been enough to allay this terminological problem, since the authors keep on using the terms with both meanings. Thus, a first goal of this tutorial is to clarify the difference between both terms. In addition, the chemical approaches for food authentication, i.e., chemical markers, component profiling and instrumental fingerprinting, have been described. A new term, designated as 'food identitation', has been introduced in order to complete the life cycle of the chemical-based food authentication process. Chromatographic fingerprinting has been explained in detail and some strategies which could be applied has been clarified and discussed. Particularly, the strategies for chromatographic signals acquisition and chromatographic data handling are unified in a single framework. Finally, an overview about the applications of chromatographic (GC and LC) fingerprints in food authentication using different chemometric techniques has been included.

  18. Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids.

    PubMed

    Acevska, J; Stefkov, G; Petkovska, R; Kulevanova, S; Dimitrovska, A

    2012-05-01

    The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)-high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the "green trend" of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

  19. QSAR models for prediction of chromatographic behavior of homologous Fab variants.

    PubMed

    Robinson, Julie R; Karkov, Hanne S; Woo, James A; Krogh, Berit O; Cramer, Steven M

    2016-12-12

    While quantitative structure activity relationship (QSAR) models have been employed successfully for the prediction of small model protein chromatographic behavior, there have been few reports to date on the use of this methodology for larger, more complex proteins. Recently our group generated focused libraries of antibody Fab fragment variants with different combinations of surface hydrophobicities and electrostatic potentials, and demonstrated that the unique selectivities of multimodal resins can be exploited to separate these Fab variants. In this work, results from linear salt gradient experiments with these Fabs were employed to develop QSAR models for six chromatographic systems, including multimodal (Capto MMC, Nuvia cPrime, and two novel ligand prototypes), hydrophobic interaction chromatography (HIC; Capto Phenyl), and cation exchange (CEX; CM Sepharose FF) resins. The models utilized newly developed "local descriptors" to quantify changes around point mutations in the Fab libraries as well as novel cluster descriptors recently introduced by our group. Subsequent rounds of feature selection and linearized machine learning algorithms were used to generate robust, well-validated models with high training set correlations (R(2)  > 0.70) that were well suited for predicting elution salt concentrations in the various systems. The developed models then were used to predict the retention of a deamidated Fab and isotype variants, with varying success. The results represent the first successful utilization of QSAR for the prediction of chromatographic behavior of complex proteins such as Fab fragments in multimodal chromatographic systems. The framework presented here can be employed to facilitate process development for the purification of biological products from product-related impurities by in silico screening of resin alternatives. Biotechnol. Bioeng. 2016;9999: 1-10. © 2016 Wiley Periodicals, Inc.

  20. Qualitative evaluation of chromatographic data from quality control schemes using a support vector machine.

    PubMed

    Ventura, M; Sanchez-Niubo, A; Ruiz, F; Agell, N; Ventura, R; Angulo, C; Domingo-Salvany, A; Segura, J; Torre, R de la

    2008-01-01

    The qualitative evaluation of chromatographic data in the framework of external quality assurance schemes is considered in this paper. The homogeneity in the evaluation of chromatographic data among human experts in samples with analytes close to the limit of detection of analytical methods was examined and also a Support Vector Machine (SVM) was developed as an alternative to experts for a more homogeneous and automatic evaluation. A set of 105 ion chromatograms obtained by anti-doping control laboratories was used in this study. The quality of the ion chromatograms was evaluated qualitatively by nine independent experts (associating a score from 0 to 4) and also more objectively taking into account chromatographic parameters (peak width, asymmetry, resolution and S/N ratio). Results obtained showed a high degree of variability among experts when judging ion chromatograms. Experts applying extremely outlying evaluation criteria were identified and excluded from the data used to develop the SVM. This machine was built providing the system with qualitative information (scores assigned by experts) and with objective data (parameters) of the ion chromatograms. A seven-fold cross-validation approach was used to train and to evaluate the predictive ability of the machine. According to the results obtained, the SVM developed was found to be close to the reasoning process followed by the homogeneous human expert group. This machine also could provide a scoring system to sort laboratories according to the quality of their results. The qualitative evaluation of analytical records using a scoring system allowed the identification of the main factors affecting the quality of chromatographic analytical data, such as the specific analytical technique applied and the adherence to guidelines for reporting positive results.