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Sample records for on-line bead-injection preconcentration

  1. Automated on-line renewable solid-phase extraction-liquid chromatography exploiting multisyringe flow injection-bead injection lab-on-valve analysis.

    PubMed

    Quintana, José Benito; Miró, Manuel; Estela, José Manuel; Cerdà, Víctor

    2006-04-15

    In this paper, the third generation of flow injection analysis, also named the lab-on-valve (LOV) approach, is proposed for the first time as a front end to high-performance liquid chromatography (HPLC) for on-line solid-phase extraction (SPE) sample processing by exploiting the bead injection (BI) concept. The proposed microanalytical system based on discontinuous programmable flow features automated packing (and withdrawal after single use) of a small amount of sorbent (<5 mg) into the microconduits of the flow network and quantitative elution of sorbed species into a narrow band (150 microL of 95% MeOH). The hyphenation of multisyringe flow injection analysis (MSFIA) with BI-LOV prior to HPLC analysis is utilized for on-line postextraction treatment to ensure chemical compatibility between the eluate medium and the initial HPLC gradient conditions. This circumvents the band-broadening effect commonly observed in conventional on-line SPE-based sample processors due to the low eluting strength of the mobile phase. The potential of the novel MSFI-BI-LOV hyphenation for on-line handling of complex environmental and biological samples prior to reversed-phase chromatographic separations was assessed for the expeditious determination of five acidic pharmaceutical residues (viz., ketoprofen, naproxen, bezafibrate, diclofenac, and ibuprofen) and one metabolite (viz., salicylic acid) in surface water, urban wastewater, and urine. To this end, the copolymeric divinylbenzene-co-n-vinylpyrrolidone beads (Oasis HLB) were utilized as renewable sorptive entities in the micromachined unit. The automated analytical method features relative recovery percentages of >88%, limits of detection within the range 0.02-0.67 ng mL(-1), and coefficients of variation <11% for the column renewable mode and gives rise to a drastic reduction in operation costs ( approximately 25-fold) as compared to on-line column switching systems. PMID:16615800

  2. On-line preconcentration strategies for analyzing pesticides in fruits and vegetables by micellar electrokinetic chromatography.

    PubMed

    Juan-García, Ana; Font, Guillermina; Picó, Yolanda

    2007-06-15

    Five pesticides (fludioxonil, procymidone, pyriproxyfen, dinoseb and carbendazim) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 20 mmol l(-1) phosphate buffer at pH 2.3, containing 25 mmol l(-1) sodium dodecylsulfate and 10% methanol. Three on-line concentration strategies, sweeping (SW), normal stacking with reversed migration and a water plug (SRW) and stacking with reverse migration and removal of sample matrix using polarity switching (SRMM), were compared. About 10-, 30- and 50-fold increases in detection sensitivity, compared with standard hydrodynamic injection (5 s at 0.5 psi), were observed with SW, SRW and SRMM, respectively. Limits of detection (LODs) ranged from 0.002 to 0.03 microg ml(-1) using only the on-line preconcentration procedures without any off-line concentration of the extract. A solid-phase extraction (SPE) procedure, for previous isolation and concentration of the analytes, was used in combination with any of the proposed on-line preconcentration strategies, which achieves the determination of pesticides at limits of quantification (LOQs) lower than 0.01 mg kg(-1). The recoveries obtained by SPE in samples spiked at 0.01 mg kg(-1) were between 70 and 100%, with RSDs between 10 and 18% using SRMM. Samples of fruits and vegetables were taken from the market, extracted by the proposed procedure and analyzed with RM-MEKC with the on-line strategies. PMID:17306816

  3. Development of an on-line preconcentration system for zinc determination in biological samples.

    PubMed

    Dutra, Rosilene L; Maltez, Heloisa F; Carasek, Eduardo

    2006-04-15

    An on-line preconcentration system for zinc determination in 24-h urine, blood plasma and erythrocyte matrices by flame atomic absorption spectrometry (FAAS) was used. This procedure was based on adsorption of Zn(II) ions onto a minicolumn filled with silica gel, chemically modified with niobium(V) oxide (Nb(2)O(5)-SiO(2)). The determination of the optimum conditions for Zn(II) preconcentration was done using two-level full factorial and Doehlert designs. In the optimization procedure, four variables (sample pH, eluent concentration, sample flow rate and eluent flow rate) were investigated. The results obtained from the full factorial design demonstrated that the sample pH and sample flow rate variables, and their interactions, were statistically significant. A Doehlert matrix was used in order to determine the optimum conditions for the sample pH and sample flow rate. The optimized conditions for sample pH and flow rate sampling were 6.6 and 7.1 ml min(-1), respectively, to obtain the maximum Zn(II) preconcentration and determination in the biological samples studied. Parameters of analytical curve, precision, effect of other ions in the proposed system and accuracy were achieved to assess the proposed method. The accuracy was confirmed by analysis of certified reference materials (urine Seronorm Trace Elements) and recovery tests in blood plasma and erythrocyte samples. Detection limit (3sigma/S) of 0.77 microg l(-1), precision (calculated as relative standard deviation) of 1.5% for Zn(II) concentration of 10 microg l(-1) (n=7) and a sampling frequency of 27 samples/h were obtained from the proposed system. PMID:18970593

  4. Analysis of acrylamide in food products by microchip electrophoresis with on-line multiple-preconcentration techniques.

    PubMed

    Wu, Minglei; Chen, Wujuan; Wang, Guan; He, Pingang; Wang, Qingjiang

    2016-10-15

    In this paper, a microchip electrophoresis method based on on-line multiple-preconcentration techniques combining field-amplified sample stacking and reversed-field stacking was developed for highly efficient analysis of acrylamide in food products. The related mechanism as well as important parameters governing separation and preconcentration have been investigated in order to obtain maximum resolution and sensitivity. The best separation was achieved using a 100mM borate solution at pH 9.3 as running buffer, and a sensitivity enhancement factor of 432 was obtained using this concentration method under optimal conditions. The detection limit of acrylamide was 1ng/mL, which was comparable to those previously obtained using CE methods with on-line preconcentration techniques and was 41-700 times lower than those previously reported CE methods without concentration process. The proposed method also gave satisfactory and reliable results in the analysis of acrylamide in potato chips and French fries.

  5. Ionic liquids in enhancing the sensitivity of capillary electrophoresis: Off-line and on-line sample preconcentration techniques.

    PubMed

    El-Hady, Deia Abd; Albishri, Hassan M; Wätzig, Hermann

    2016-07-01

    The popularity of ionic liquids (ILs) has grown during the last decade in enhancing the sensitivity of CE through different off-line or on-line sample preconcentration techniques. Water-insoluble ILs were commonly used in IL-based liquid phase microextraction, in all its variants, as off-line sample preconcentration techniques combined with CE. Water-soluble ILs were rarely used in IL-based aqueous two phase system (IL-ATPS) as an off-line sample preconcentration approach combined with CE in spite of IL-ATPS predicted features such as more compatibility with CE sample injection due to its relatively low viscosity and more compatibility with CE running buffers avoid, in some cases, anion exchange precipitation. Therefore, the attentions for the key parameters affecting the performance of IL-ATPSs were generally presented and discussed. On-line CE preconcentration techniques containing IL-based surfactants at nonmicellar or micellar concentrations have become another interesting area to improve CE sensitivity and it is likely to remain a focus of the field in the endeavor because of their numerous to create rapid, simple and sensitive systems. In this article, significant contributions of ILs in enhancing the sensitivity of CE are described, and a specific overview of the relevant examples of their applications is also given. PMID:27067143

  6. On-line preconcentration and chiral separation of propiconazole by cyclodextrin-modified micellar electrokinetic chromatography.

    PubMed

    Wan Ibrahim, Wan Aini; Hermawan, Dadan; Sanagi, Mohd Marsin

    2007-11-01

    A method for the chiral separation of propiconazole using cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC) with hydroxypropyl-gamma-cyclodextrin (HP-gamma-CD) as chiral selector is reported. The use of a mixture of 30 mM HP-gamma-CD, 50mM SDS, methanol-acetonitrile 10%:5% (v/v) in 25 mM phosphate buffer solution was able to separate two enantiomeric pairs of propiconazole. Stacking- and sweeping-CD-MEKC under neutral pH (pH 7) and under acidic condition (pH 3.0) were used as two on-line preconcentration methods to increase detection sensitivity of propiconazole. Good repeatabilities in the migration time, peak area and peak height were obtained in terms of relative standard deviation (RSD). A sensitivity enhancement factor of 100-fold was achieved using sweeping-CD-MEKC at acidic pH. This is the first report on the separation of two pairs of propiconazole enantiomers and all the enantiomers of fenbuconazole and tebuconazole using sweeping-CD-MEKC. The limit of detection (S/N=3) for the three triazole fungicides ranged from 0.09 to 0.1 microg/mL, which is well below the maximum residue limits (MRL) set by Codex Alimentarius Commission (CAC). Combination of solid-phase extraction (SPE) pretreatment and sweeping-CD-MEKC procedure was applied to the determination of selected triazole fungicides in grapes samples spiked at concentration 10-40 times lower than the MRL established by the CAC. The average recoveries of the selected fungicides in spiked grapes samples were good, ranging from 73% to 109% with RSD of 9-12% (n=3).

  7. On-line preconcentration and determination of chromium in parenteral solutions by flow injection-flame atomic absorption spectrometry.

    PubMed

    Wuilloud, Gustavo M; Wuilloud, Rodolfo G; de Wuilloud, Jorgelina C A; Olsina, Roberto A; Martinez, Luis D

    2003-02-01

    An on-line chromium preconcentration and determination system implemented with flame atomic absorption spectrometry (FAAS) associated to flow injection (FI) was studied. For the retention of chromium, 4-(2-Thiazolylazo)-resorcinol (TAR) and Amberlite XAD-16 were used, at pH 5.0. The Cr-TAR complex was removed from the micro-column with ethanol. An enrichment factor of 50 was obtained for the preconcentration of 50 ml of sample solution. The detection limit value for the preconcentration of 50 ml of aqueous solution of Cr was 20 ng l(-1). The precision for ten replicate determinations at the 5 microg l(-1) Cr levels was 2.9% relative standard deviation (RSD), calculated from the peak heights obtained. The calibration graph using the preconcentration system for chromium was linear with a correlation coefficient of 0.9997 at levels near the detection limits up to at least 100 microg l(-1). The method was successfully applied to the determination of chromium in parenteral solution samples.

  8. Single-step enantioselective amino acid flux analysis by capillary electrophoresis using on-line sample preconcentration with chemical derivatization.

    PubMed

    Ptolemy, Adam S; Tran, Lara; Britz-McKibbin, Philip

    2006-07-15

    Capillary electrophoresis (CE) represents a versatile platform for integrating sample pretreatment with chemical analysis because of its ability to tune analyte electromigration and band dispersion properties in discontinuous electrolyte systems. In this article, a single-step method that combines on-line sample preconcentration with in-capillary chemical derivatization is developed for rapid, sensitive, and enantioselective analysis of micromolar levels of amino acids that lack intrinsic chromophores by CE with UV detection. Time-resolved electrophoretic studies revealed two distinct stages of amino acid band narrowing within the original long sample injection plug occurring both prior to and after in-capillary labeling via zone passing by ortho-phthalaldehyde/N-acetyl l-cysteine (OPA/NAC). This technique enabled direct analysis of d-amino acids in a 95% enantiomeric excess mixture with sub-micromolar detection limits and minimal sample handling, where the capillary functions as a preconcentrator, microreactor, and chiral selector. On-line sample preconcentration with chemical derivatization CE (SPCD-CE) was applied to study the enantioselective amino acid flux in Escherichia coli bacteria cultures, which demonstrated a unique l-Ala efflux into the extracellular medium. New strategies for high-throughput analyses of low-abundance metabolites are important for understanding fundamental physiological processes in bacteria required for screening the efficacy of new classes of antibiotics as well as altered metabolism in genetically modified mutant strains.

  9. Single-step enantioselective amino acid flux analysis by capillary electrophoresis using on-line sample preconcentration with chemical derivatization.

    PubMed

    Ptolemy, Adam S; Tran, Lara; Britz-McKibbin, Philip

    2006-07-15

    Capillary electrophoresis (CE) represents a versatile platform for integrating sample pretreatment with chemical analysis because of its ability to tune analyte electromigration and band dispersion properties in discontinuous electrolyte systems. In this article, a single-step method that combines on-line sample preconcentration with in-capillary chemical derivatization is developed for rapid, sensitive, and enantioselective analysis of micromolar levels of amino acids that lack intrinsic chromophores by CE with UV detection. Time-resolved electrophoretic studies revealed two distinct stages of amino acid band narrowing within the original long sample injection plug occurring both prior to and after in-capillary labeling via zone passing by ortho-phthalaldehyde/N-acetyl l-cysteine (OPA/NAC). This technique enabled direct analysis of d-amino acids in a 95% enantiomeric excess mixture with sub-micromolar detection limits and minimal sample handling, where the capillary functions as a preconcentrator, microreactor, and chiral selector. On-line sample preconcentration with chemical derivatization CE (SPCD-CE) was applied to study the enantioselective amino acid flux in Escherichia coli bacteria cultures, which demonstrated a unique l-Ala efflux into the extracellular medium. New strategies for high-throughput analyses of low-abundance metabolites are important for understanding fundamental physiological processes in bacteria required for screening the efficacy of new classes of antibiotics as well as altered metabolism in genetically modified mutant strains. PMID:16753129

  10. Analysis of acrylamide in food products by microchip electrophoresis with on-line multiple-preconcentration techniques.

    PubMed

    Wu, Minglei; Chen, Wujuan; Wang, Guan; He, Pingang; Wang, Qingjiang

    2016-10-15

    In this paper, a microchip electrophoresis method based on on-line multiple-preconcentration techniques combining field-amplified sample stacking and reversed-field stacking was developed for highly efficient analysis of acrylamide in food products. The related mechanism as well as important parameters governing separation and preconcentration have been investigated in order to obtain maximum resolution and sensitivity. The best separation was achieved using a 100mM borate solution at pH 9.3 as running buffer, and a sensitivity enhancement factor of 432 was obtained using this concentration method under optimal conditions. The detection limit of acrylamide was 1ng/mL, which was comparable to those previously obtained using CE methods with on-line preconcentration techniques and was 41-700 times lower than those previously reported CE methods without concentration process. The proposed method also gave satisfactory and reliable results in the analysis of acrylamide in potato chips and French fries. PMID:27173547

  11. An on-line preconcentration/separation system for the determination of bismuth in environmental samples by FAAS.

    PubMed

    Sahan, Serkan; Saçmaci, Serife; Sahin, Uğur; Ulgen, Ahmet; Kartal, Senol

    2010-03-15

    An on-line preconcentration procedure for the determination of bismuth by flame atomic absorption spectrometry (FAAS) has been described. Lewatit TP-207 chelating resin, including iminodiacetate group, packed in a minicolumn was used as adsorbent material. Bi(III) was sorbed on the chelating resin, from which it could be eluted with 3 mol L(-1) HNO(3) and then introduced directly to the nebulizer-burner system of FAAS. Best preconcentration conditions were established by testing different resin quantities, acidity of sample, types of eluent, sample and eluent solution volumes, adsorption and elution flow rates, and effect of interfering ions. The detection limit of the method was 2.75 microg L(-1) while the relative standard deviation was 3.0% for 0.4 microg mL(-1) Bi(III) concentration. The developed method has been applied successfully to the determination of bismuth in pharmaceutical cream, standard reference materials and various natural water samples with satisfactory results.

  12. New advances in on-line sample preconcentration by capillary electrophoresis using dynamic pH junction.

    PubMed

    Ptolemy, Adam S; Britz-McKibbin, Philip

    2008-12-01

    The small injection volumes and narrow dimensions characteristic of microseparation techniques place constraints on concentration sensitivity that is required for trace chemical analyses. On-line sample preconcentration techniques using dynamic pH junction and its variants have emerged as simple yet effective strategies for enhancing concentration sensitivity of weakly ionic species by capillary electrophoresis (CE). Dynamic pH junction offers a convenient format for electrokinetic focusing of dilute sample plugs directly in-capillary for improved detection without off-line sample pretreatment. In this report, we highlight new advances in dynamic pH junction which have been reported to enhance method performance while discussing challenges for future research.

  13. An automated on-line minicolumn preconcentration cold vapour atomic absorption spectrometer: application to determination of cadmium in water samples.

    PubMed

    Sahan, Serkan; Sahin, Uğur

    2012-01-15

    A method was developed for on-line solid phase preconcentration and cold vapour atomic absorption spectrometric determination of Cd(II) in aqueous samples. Lewatit Monoplus TP207 iminodiacetate chelating resin was used for the separation and preconcentration of Cd(II) ions at pH 4.0. The whole system was labmade. The influence of analytical parameters such as concentration of eluent and sodium tetrahydroborate solution, flow rate of eluent, sample, and Ar, and matrix ions were investigated. A preconcentration factor of 20 and a detection limit (3s(b)) of 2.1ngL(-1), along with a sampling frequency of 28h(-1) were achieved with 1.4min of sample loading time and with 2.8mL sample consumption. The relative standard deviation (R.S.D.) was 2.5% for 0.05μgL(-1) Cd(II) level. The developed method was used for Cd(II) analysis in water samples. The certified reference material (LGC6019) experimental results are in good agreement with the certified value.

  14. Capability of diatomaceous earth to preconcentrate and store Pb and Cr: on-line determination by FI-FAAS.

    PubMed

    Cabañero, Isabel; Madrid, Yolanda; Cámara, Carmen

    2002-07-01

    The diatomaceous earth (DE) has an important ability to retain metals such as Cd, Cr, Mn and Pb, which can be used for their stabilization in the environment and for analytical purposes. In this paper a fast on-line preconcentration method for the determination of Cr and Pb in waters by flow injection flame atomic absorption spectrometry is described. Preconcentration was based on the retention of Cr and Pb on a DE immobilized in silica gel at pH 3.0 and subsequent elution with 200 microL of 3 mol L(-1) HCl. The preconcentration factors were 100 and 150 for Pb and Cr respectively, for 16 mL water sample volume. The detection limits under these conditions were 3 ng mL(-1) and 1 ng mL(-1) for Pb and Cr, respectively. The stability of Cr and Pb retained on silica gel-DE columns was established. Silica gel-DE microcolumns with the retained analytes were stored for 2 months at two different temperatures: 4 degrees C and room temperature. At regular time intervals, both metals were eluted and quantified. The results showed the potential of the procedure for sampling and storing water samples for subsequent metal determination, avoiding the problems associated with maintaining species integrity in aqueous solution, and the possibility to of decontaminating polluted spaces.

  15. On-line preconcentration of fluorescent derivatives of catecholamines in cerebrospinal fluid using flow-gated capillary electrophoresis.

    PubMed

    Zhang, Qiyang; Gong, Maojun

    2016-06-10

    Flow-gated capillary electrophoresis (CE) coupled with microdialysis has become an important tool for in vivo bioanalytical measurements because it is capable of performing rapid and efficient separations of complex biological mixtures thus enabling high temporal resolution in chemical monitoring. However, the limit of detection (LOD) is often limited to a micro- or nano-molar range while many important target analytes have picomolar or sub-nanomolar levels in brain and other tissues. To enhance the capability of flow-gated CE for catecholamine detection, a novel and simple on-line sample preconcentration method was developed exclusively for fluorescent derivatives of catecholamines that were fluorogenically derivatized with naphthalene-2,3-dicarboxaldehyde (NDA) in the presence of cyanide. The effective preconcentration coupled with the sensitive laser-induced fluorescence (LIF) detection lowered the LOD down to 20pM for norepinephrine (NE) and 50pM for dopamine (DA) at 3-fold of S/N ratio, and the signal enhancement was estimated to be over 100-fold relative to normal injection when standard analytes were dissolved in artificial cerebrospinal fluid (aCSF). The basic focusing principle is novel since the sample plug contains borate while the background electrolyte (BGE) is void of borate. This strategy took advantage of the complexation between diols and borate, through which one negative charge was added to the complex entity. The sample derivatization mixture was electrokinetically injected into a capillary via the flow-gated injection, and then NE and DA derivatives were selectively focused to a narrow zone by the reversible complexation. Separation of NE and DA derivatives was executed by incoming surfactants of cholate and deoxycholate mixed in the front BGE plug. This on-line preconcentration method was finally applied to the detection of DA in rat cerebrospinal fluid (CSF) via microdialysis and on-line derivatization. It is anticipated that the method would

  16. Determination of lead in sea-water with a graphite furnace atomic absorption spectrometer and an improved automatic on-line pre-concentration system

    NASA Astrophysics Data System (ADS)

    Liu, Zhen-Shan; Huang, Shang-Da

    1995-03-01

    An improved automatic on-line pre-concentration system for graphite furnace atomic absorption spectrometry (GFAAS) for the determination of trace metals in sea-water was developed. This system was modified from a Perkin-Elmer AS-40 autosampler by mounting a silica gel C 18 microcolumn near the tip of the autosampler capillary. The pre-concentration procedure was performed by using a four-way distribution valve and controlled by a programmable controller. The pre-concentration system developed previously was improved by using a peristaltic pump to replace the reciprocating pumps, a newly designed tube bed adjuster to release the back-pressure in the pre-concentration system, and a better control program, such that on-line pre-concentration became more reliable and fully automatic. The chelating agent ammonium pyrolidinedithiocarbamate (APDC) and a miniature column packed with 5 mg of C 18 silica gel were used for pre-concentration. This system was tested by analyzing the lead content in reference standard sea-water samples. A sample volume of only 2 ml was required to determine lead in sea-water. The relative limit of detection of lead was 3.5 pg/ml.

  17. Automated on-line preconcentration of palladium on different sorbents and its determination in environmental samples.

    PubMed

    Sánchez Rojas, Fuensanta; Bosch Ojeda, Catalina; Cano Pavón, José Manuel

    2007-01-01

    The determination of noble metals in environmental samples is of increasing importance. Palladium is often employed as a catalyst in chemical industry and is also used with platinum and rhodium in motor car catalytic converters which might cause environmental pollution problems. Two different sorbents for palladium preconcentration in different samples were investigated: silica gel functionalized with 1,5-bis(di-2-pyridyl)methylene tbiocarbohydrazide (DPTH-gel) and [1,5-Bis(2-pyridyl)-3-sulphophenyI methylene thiocarbonohydrazide (PSTH) immobilised on an anion-exchange resin (Dowex lx8-200)]. The sorbents were tested in a micro-column, placed in the auto-sampler arm, at the flow rate 2.8 mL min(-1). Elution was performed with 4 M HCl and 4 M HNO3, respectively. Satisfactory results were obtained for two sorbents.

  18. Use of Muromac A-1 chelating resin for determination of copper and molybdenum in seawater by atomic absorption with on-line preconcentration

    NASA Astrophysics Data System (ADS)

    Sung, Yu-Hsiang; Liu, Zhen-Shan; Huang, Shang-Da

    1997-06-01

    Muromac A-1 chelating resin is used to preconcentrate trace metals (copper and molybdenum) in seawater. A miniature column (4-7 μl) packed with resin and a home-made automatic on-line preconcentration system for graphite furnance atomic absorption spectrometry (GFAAS) were used. This preconcentration system was modified from a Perkin-Elmer AS-40 autosampler by mounting a Muromac A-1 microcolumn near the tip of the autosampler capillary. The preconcentration procedure was performed by using a four-way distribution valve and a programmable controller. A sample volume of only 20-200 μl was required for determining copper and molybdenum in seawater. The calibration graph method was used; the detection limits for copper and molybdenum were 0.05 ppb and 0.25 ppb respectively. The sample throughput was 18-26 h -1. The accuracy of the method was confirmed by the analysis of certified reference saline waters.

  19. New advances in on-line sample preconcentration by capillary electrophoresis using dynamic pH junction.

    PubMed

    Ptolemy, Adam S; Britz-McKibbin, Philip

    2008-12-01

    The small injection volumes and narrow dimensions characteristic of microseparation techniques place constraints on concentration sensitivity that is required for trace chemical analyses. On-line sample preconcentration techniques using dynamic pH junction and its variants have emerged as simple yet effective strategies for enhancing concentration sensitivity of weakly ionic species by capillary electrophoresis (CE). Dynamic pH junction offers a convenient format for electrokinetic focusing of dilute sample plugs directly in-capillary for improved detection without off-line sample pretreatment. In this report, we highlight new advances in dynamic pH junction which have been reported to enhance method performance while discussing challenges for future research. PMID:19082065

  20. Determination of phenolic acids in plant extracts using CZE with on-line transient isotachophoretic preconcentration.

    PubMed

    Honegr, Jan; Pospíšilová, Marie

    2013-02-01

    A novel transient ITP-CZE for preconcentration and determination of seven phenolic acids (caffeic acid, cinnamic acid, p-coumaric acid, ferulic acid, protocatechuic acid, syringic acid, and vanilic acid) was developed and validated. Effects of several factors such as control of EOF, pH and buffer concentration, addition of organic solvents and CDs, and conditions for sample injection were investigated. Sample self-stacking was applied by means of induction of transient ITP, which was realized by adding sodium chloride into the sample. The CZE was realized in 200 mM borate buffer ((w)(s)pH 9.2) containing 37.5% methanol, 0.001% hexadimethrine bromide, and 15 mM 2-hydroxypropyl-β-CD. Under the optimal conditions for analysis, analytes were separated within 20 min. Linearity was tested for each compound in the concentration range of 0.1-10 μg/mL (R = 0.9906-0.9968) and the detection limits (S/N = 3) ranged from 11 ng/mL (protocatechuic acid) to 31 μg/mL (syringic acid). The validated method was applied to the ethanolic extract of Epilobium parviflorum, Onagraceae. The method of SPE was used for the precleaning of the sample. PMID:23401390

  1. The Trace Analysis of DEET in Water using an On-line Preconcentration Column and Liquid Chromatography with UV Photodiode Array Detection

    EPA Science Inventory

    A method for the detection of trace levels of N,N-diethyl-m-toluamide (DEET) in water is discussed. The method utilizes an on-line preconcentration column in series with high performance liquid chromatography (HPLC) and UV photodiode array detection. DEET, a common insect repel...

  2. Sensitive simultaneous determination of three sulfanilamide artificial sweeters by capillary electrophoresis with on-line preconcentration and contactless conductivity detection.

    PubMed

    Yang, Lirong; Zhou, ShengJi; Xiao, Yuezhou; Tang, Yufeng; Xie, Tianyao

    2015-12-01

    A sensitive method followed by capillary electrophoresis with on-line perconcentration and capacitively coupled contactless conductivity detection (CE-C(4)D) was evaluated as a novel approach for the determination of three sulfanilamide artificial sweeteners (acesulfame-K, sodium saccharin and sodium cyclamate) in beverages. The on-line preconcentration technique, namely field-amplified sample injection, coupled with CE-C(4)D were successfully developed and optimized. The separation was achieved within 10 min under the following conditions: an uncoated fused-silica capillary (45 cm × 50 μm i.d., Leff=40 cm), 20 mmol L(-1) HAc as running buffer, separation voltage of -12 kV, electrokinetic injection of -11 kV × 8 s. The detection limits of acesulfame-K, sodium saccharin and sodium cyclamate were 4.4, 6.7 and 8.8 μg L(-1), respectively. The relative standard deviation varied in the range of 3.0-5.0%. Results of this study show a great potential method for the fast screening of these artificial sweeteners contents in commercial beverages. PMID:26041216

  3. Further study on a flow injection on-line multiplexed sorption preconcentration coupled with flame atomic absorption spectrometry for trace element determination.

    PubMed

    Li, Yan; Jiang, Yan; Yan, Xiu-Ping

    2004-10-20

    A further study on a newly developed flow injection (FI) on-line multiplexed sorption preconcentration (MSP) using a knotted reactor coupled with flame atomic absorption spectrometry (FAAS) was carried out to demonstrate its applicability and limitation for trace element determination. For this purpose, Cr(VI), Cu(II), Ni(II) and Co(II) were selected as the analytes, and detailed comparison was made between the MSP-FAAS and conventional FI on-line sorption preconcentration FAAS in respect to retention efficiency and linear ranges of absorbance versus sample loading flow rate and total preconcentration time. Introduction of an air-flow for removal of the residual solution in the KR after each sub-injection in the MSP procedure played a decisive role in the improvement of retention efficiency. The linearity of absorbance versus sample loading flow rate or total preconcentration time was extended to a more degree for the metal ions with less stability of their PDC (pyrrolidine dithiocarbamate) complexes than those with more stable PDC complexes. It seems that the MSP procedure behaves advantages beyond the inflection points in the diagrams of absorbance versus total preconcentration time and sample loading flow rate obtained by conventional (a single continuous) preconcentration procedure. With a sample loading flow rate of 6.0mlmin(-1) and a total preconcentration time of 180s, the retention efficiencies were increased from 25, 46, 41 and 63% with a single continuous sorption preconcentration to 44, 78, 65 and 75% with a six sub-injection preconcentration procedure for Cr(VI), Co(II), Ni(II), and Cu(II), respectively. The detection limits were 0.40, 0.33, 0.31 and 0.26mugl(-1) for Cr(VI), Co(II), Ni(II), and Cu(II), respectively. The precision (R.S.D.) for eleven replicate determination of 2mugl(-1) Cr(VI), Co(II) and Ni(II), and 1mugl(-1) Cu(II), was 2.1, 4.1, 2.6 and 1.7%, respectively. PMID:18969669

  4. Dithizone immobilized silica gel on-line preconcentration of trace copper with detection by flame atomic absorption spectrometry.

    PubMed

    Yu, Hong-Mei; Song, Hua; Chen, Ming-Li

    2011-07-15

    A novel adsorbent-silica gel bound dithizone (H(2)Dz-SG) was prepared and used as solid-phase extraction of copper from complex matrix. The H(2)Dz-SG is investigated by means of FT-IR spectra and the SEM images, demonstrating the bonding of dithizone. The H(2)Dz-SG quantitatively adsorb copper ions, and the retained copper is afterwards collected by elution of 10% (v/v) nitric acid. An on-line flow injection solid-phase extraction procedure was developed for trace copper separation and preconcentration with detection by flame atomic spectrometry. By loading 5.4 mL of sample solution, a liner range of 0.5-120 μg L(-1), an enrichment factor of 42.6, a detection limit of 0.2 μg L(-1) and a precision of 1.7% RSD at the 40 μg L(-1) level (n=11) were obtained, along with a sampling frequency of 47 h(-1). The dynamic sorption capacity of H(2)Dz-SG to Cu(2+) was 0.76 mg g(-1). The accuracy of the proposed procedure was evaluated by determination of copper in reference water sample. The potential applications of the procedure for extraction of trace copper were successfully accomplished in water samples (tap, rain, snow, sea and river). The spiking recoveries within 91-107% are achieved. PMID:21645750

  5. Determination of heavy metals by inductively coupled plasma mass spectrometry after on-line separation and preconcentration

    NASA Astrophysics Data System (ADS)

    Dressler, Valderi L.; Pozebon, Dirce; Curtius, Adilson J.

    1998-10-01

    A method for the determination of Cu, As, Se, Cd, In, Hg, Tl, Pb and Bi in waters and in biological materials by inductively coupled plasma mass spectrometry, after an on-line separation, is described. The matrix separation and analyte preconcentration is accomplished by retention of the analytes complexed with the ammonium salt of O,O-diethyl dithiophosphoric acid in a HNO 3 solution on C 18 immobilized on silica in a minicolumn. Methanol, as eluent, is introduced in the conventional pneumatic nebulizer of the instrument. In order to use the best compromise conditions, concerning the ligand and acid concentrations, the analytes were determined in two separate groups. The enrichment factors were in the range from 5 to 61, depending on the analyte. The limits of detection varied from 0.43 ng L -1 for Bi to 33 ng L -1 for Cu. The sample consumption is only 2.3 mL for each group and the sampling frequency is 21 h -1. The accuracy was tested by analysing five certified reference materials: water, riverine water, urine, bovine muscle and bovine liver. The agreement between obtained and certified concentrations was very good, except for As. The relatively small volume of methanol, used as eluent, minimizes the problems produced by the introduction of organic solvent into the plasma.

  6. Application of capillary electrophoresis with electrokinetic supercharging and sweeping for the on-line preconcentration of phenolic acids.

    PubMed

    Lin, Yi-Hui; Huang, Hsin-Chieh; Hsu, Wan-Ling

    2015-09-01

    Phenolic acids are natural antioxidants. Many studies have confirmed that these compounds can reduce the risk of developing chronic diseases such as diabetes, cardiovascular diseases, and certain cancers. In this work, we developed a rapid and efficient capillary electrophoresis method with an on-line preconcentration technique that could be used to simultaneously analyze 10 commonly found phenolic acids in plants. Briefly, phosphate buffer solution (pH 2) was filled into an uncoated fused silica capillary as the leading electrolyte, and then samples which were prepared in borate buffer (as the terminating ion) were loaded by electrokinetic injection (-10 kV, 900 s). After sample injection, both ends of the capillary were switched to the vial containing phosphate buffer with sodium dodecyl sulfate. The separation was then performed in micellar electrokinetic chromatography (MEKC) mode at -20 kV. During the method validation, the correlation coefficient of the regression curve was measured as greater than 0.997 and the relative standard deviation and relative error were lower than 9.63 % and 4.7 %, respectively. The limits of detection (LODs, S/N = 3) of these 10 analytes ranged from 0.01 to 2.5 ng/mL. Compared with the conventional capillary zone electrophoresis (CZE) method, the sensitivity for the analytes could be increased up to 25,000-fold. The method that we developed here was applied successfully to the detection of phenolic acids in fruit juices. PMID:26159571

  7. Dithizone immobilized silica gel on-line preconcentration of trace copper with detection by flame atomic absorption spectrometry.

    PubMed

    Yu, Hong-Mei; Song, Hua; Chen, Ming-Li

    2011-07-15

    A novel adsorbent-silica gel bound dithizone (H(2)Dz-SG) was prepared and used as solid-phase extraction of copper from complex matrix. The H(2)Dz-SG is investigated by means of FT-IR spectra and the SEM images, demonstrating the bonding of dithizone. The H(2)Dz-SG quantitatively adsorb copper ions, and the retained copper is afterwards collected by elution of 10% (v/v) nitric acid. An on-line flow injection solid-phase extraction procedure was developed for trace copper separation and preconcentration with detection by flame atomic spectrometry. By loading 5.4 mL of sample solution, a liner range of 0.5-120 μg L(-1), an enrichment factor of 42.6, a detection limit of 0.2 μg L(-1) and a precision of 1.7% RSD at the 40 μg L(-1) level (n=11) were obtained, along with a sampling frequency of 47 h(-1). The dynamic sorption capacity of H(2)Dz-SG to Cu(2+) was 0.76 mg g(-1). The accuracy of the proposed procedure was evaluated by determination of copper in reference water sample. The potential applications of the procedure for extraction of trace copper were successfully accomplished in water samples (tap, rain, snow, sea and river). The spiking recoveries within 91-107% are achieved.

  8. [Two steps elution method FI on-line adsorption and preconcentration coupled with FAAS for the determination of trace zinc].

    PubMed

    Wang, Zhong-yuan; Zhang, Hong-kang; Fang, Hong-da; Su, Yao-dong; Mittal, Gauri S

    2011-12-01

    A flow injection two steps elution method on-line sorption and preconcentration system coupled to flame atomic absorption spectrometry (FAAS) was developed for the determination of trace Zn in water samples. The conventional elution procedure was divided into two steps: elution procedure and detection procedure. During the elution procedure, the eluent was pumped into KR by the suction of the peristaltic pump and through PTFE tube instead of peristaltic pump tube. By the new method, the dispersion of the analyte was decreased notably, and high absorbance peak value was achieved. Because the eluent was not through the peristaltic pump tube, the peristaltic pump tube was protected from being eroded. Emptying procedure was added in order to insure the veracity and repeatability of the experiment of every time. With 60 s (sample throughput of 37 x h(-1)) of sampling at a flow rate of 6.0 mL x min(-1), an enhancement factor (EF) of 28 (higher than 9 achieved by conventional elution method) and a detection limit (3sigma) of 0.35 x L(-1) were obtained. The precision (RSD, n=11) was 2.1% at the 20 microg x L(-1) level. When 0.1% phi triethannolamine was used as masking reagent, the recovery rate was from 98.7% to 99.6%.

  9. Determination of scandium in acid mine drainage by ICP-OES with flow injection on-line preconcentration using oxidized multiwalled carbon nanotubes.

    PubMed

    Jerez, Javier; Isaguirre, Andrea C; Bazán, Cristian; Martinez, Luis D; Cerutti, Soledad

    2014-06-01

    An on-line scandium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry associated with flow injection was studied. Trace amounts of scandium were preconcentrated by sorption on a minicolumn packed with oxidized multiwalled carbon nanotubes, at pH 1.5. The retained analyte was removed from the minicolumn with 30% (v/v) nitric acid. A total enrichment factor of 225-fold was obtained within a preconcentration time of 300 s (for a 25 mL sample volume). The overall time required for preconcentration and elution of 25 mL of sample was about 6 min; the throughput was about 10 samples per hour. The value of the detection limit was 4 ng L(-1) and the precision for 10 replicate determinations at 100 ng L(-1) Sc level was 5% relative standard deviation, calculated from the peak heights obtained. The calibration graph using the preconcentration system was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 10 mg L(-1). After optimization, the method was successfully applied to the determination of Sc in an acid drainage from an abandoned mine located in the province of San Luis, Argentina.

  10. On-Line Solid-Phase Extraction Capillary Electrophoresis Mass Spectrometry for Preconcentration and Clean-Up of Peptides and Proteins.

    PubMed

    Benavente, Fernando; Medina-Casanellas, Silvia; Giménez, Estela; Sanz-Nebot, Victoria

    2016-01-01

    One of the major drawbacks of capillary electrophoresis (CE) and other microscale separation techniques, for the analysis of low abundant peptides and proteins in complex samples, are the poor concentration limits of detection. Several strategies have been developed to improve CE sensitivity. Here, we describe an on-line solid-phase extraction capillary electrophoresis mass spectrometry method with a commercial C18 sorbent for clean-up and preconcentration of neuropeptides from highly diluted biological samples.

  11. Determining ultraviolet absorbents in sunscreen products by combining direct injection with micelle collapse on-line preconcentration capillary electrophoresis.

    PubMed

    Hsiao, Wen-Yao; Jiang, Shiuh-Jen; Feng, Chia-Hsien; Wang, Shih-Wei; Chen, Yen-Ling

    2015-02-27

    The on-line preconcentration technique of analyte focusing by micelle collapse-micellar electrokinetic chromatography (AFMC-MEKC) was combined with direct injection without extraction to determine ultraviolet absorbents in sunscreen products. The stacking mechanism is based on the transport, release, and accumulation of analytes bound to micelle carriers that are collapsed into the micelle dilution zone. The following optimized conditions were determined: the running buffer was 10mM Tris buffer (pH 9.5) containing 60mM SDS, 7mM γ-CD and 20% ethanol; the SDS concentration was required to be slightly above the critical micelle concentration (cmc) value (7.4mM) in the sample matrix, which allowed the micelle dilution zone to form when voltage was applied; and finally, the sample was prepared in 100mM Tris buffer (pH 9.0) containing 7.5mM SDS and 20% (v/v) ethanol to provide sufficient resolution and to improve the sensitivity. Samples were injected at 0.5psi for 40s, and the separation voltage was set at 15kV for first 15min and then increased to 23kV to decrease the analysis time. The detection sensitivity for ultraviolet absorbents was enhanced by approximately 41-fold using AFMC-MEKC compared to conventional MEKC. The limit of detection (S/N=3) was 98nM for benzophenone-2 and benzophenone-4. The correlation of the regression curve was greater than 0.995. The relative error and relative standard deviation were lower than 9.94% with high precision and accuracy. The recoveries of nine ultraviolet absorbents in a homemade emulsion were between 95.08% and 104.57%. After optimization and validation, this AFMC-MEKC method combined with direct injection is considered to be established and successfully applicable to commercial sunscreen products.

  12. Thermospray flame furnace-AAS determination of copper after on-line sorbent preconcentration using a system optimized by experimental designs.

    PubMed

    Tarley, César Ricardo Teixeira; Figueiredo, Eduardo da Costa; Matos, Geraldo Domingues

    2005-11-01

    The present paper describes the on-line coupling of a flow-injection system to a new technique, thermospray flame furnace-AAS (TS-FF-AAS), for the preconcentration and determination of copper in water samples. Copper was preconcentrated onto polyurethane foam (PUF) complexed with ammonium O,O-diethyldithiophosphate (DDTP), while elution was performed using 80% (v/v) ethanol. An experimental design for optimizing the copper preconcentration system was established using a full factorial (2(4)) design without replicates for screening and a Doehlert design for optimization, studying four variables: sample pH, ammonium O,O-diethyldithiophosphate (DDTP) concentration, presence of a coil and the sampling flow rate. The results obtained from the full factorial and based on a Pareto chart indicate that only the pH and the DDTP concentration, as well as their interaction, exert influence on the system within a 95% confidence level. The proposed method provided a preconcentration factor of 65 fold, thus notably improving the detectability of TS-FF-AAS. The detection limit was 0.22 microg/dm3 and the precision, expressed as the relative standard deviation (RSD) for eight independent determinations, was 2.7 and 1.1 for copper solutions containing 5 and 30 microg/dm3, respectively. The procedure was successfully applied for copper determination in water samples. PMID:16317902

  13. [Determination of trace and ultra-trace level bromate in water by large volume sample injection with enrichment column for on-line preconcentration coupled with ion chromatography].

    PubMed

    Liu, Jing; He, Qingqing; Yang, Lili; Hu, Enyu; Wang, Meifei

    2015-10-01

    A method for the determination of trace and ultra-trace level bromate in water by ion chromatography with large volume sample injection for on-line preconcentration was established. A high capacity Dionex IonPac AG23 guard column was simply used as the enrichment column instead of the loop for the preconcentration of bromate. High purity KOH solution used as eluent for gradient elution was on-line produced by an eluent generator automatically. The results showed that a good linear relationship of bromate was exhibited in the range of 0.05-51.2 μg/L (r ≥ 0.999 5), and the method detection limit was 0.01 μg/L. Compared with conventional sample injection, the injection volume was up to 5 mL, and the enrichment factor of this method was about 240 times. This method was successfully applied for several real samples of pure water which were purchased in the supermarket, and the recoveries of bromate were between 90%-100% with the RSDs (n = 6) of 2.1%-6.4% at two spiked levels. This method without pretreatment is simple, and of high accuracy and precision. The preconcentration can be achieved by large volume sample injection. It is suitable for the analysis of trace and ultra-trace level bromate.

  14. Single-step analysis of low abundance phosphoamino acids via on-line sample preconcentration with chemical derivatization by capillary electrophoresis.

    PubMed

    Ptolemy, Adam S; Britz-McKibbin, Philip

    2005-09-01

    New strategies for rapid, sensitive and high-throughput analysis of low abundance metabolites in biological samples are required for future metabolomic research. In this report, a direct method for sub-micromolar analyses of phosphoamino acids was developed using on-line sample preconcentration with 9-fluorenylmethyloxycarbonyl chloride (FMOC) derivatization by capillary electrophoresis (CE) and UV detection. Analyte focusing by dynamic pH junction and FMOC labeling efficiency were influenced by several experimental factors including buffer pH, ionic strength, sample injection length and FMOC concentration. About a 200-fold enhancement in concentration sensitivity was achieved under optimal conditions relative to conventional off-line derivatization, as reflected by a detection limit (S/N approximately 3) of 0.1 microM. In-capillary sample preconcentration with chemical labeling by CE offers a unique single-step analytical platform for high-throughput screening of low abundance metabolites without intrinsic chromophores.

  15. Single-step analysis of low abundance phosphoamino acids via on-line sample preconcentration with chemical derivatization by capillary electrophoresis.

    PubMed

    Ptolemy, Adam S; Britz-McKibbin, Philip

    2005-09-01

    New strategies for rapid, sensitive and high-throughput analysis of low abundance metabolites in biological samples are required for future metabolomic research. In this report, a direct method for sub-micromolar analyses of phosphoamino acids was developed using on-line sample preconcentration with 9-fluorenylmethyloxycarbonyl chloride (FMOC) derivatization by capillary electrophoresis (CE) and UV detection. Analyte focusing by dynamic pH junction and FMOC labeling efficiency were influenced by several experimental factors including buffer pH, ionic strength, sample injection length and FMOC concentration. About a 200-fold enhancement in concentration sensitivity was achieved under optimal conditions relative to conventional off-line derivatization, as reflected by a detection limit (S/N approximately 3) of 0.1 microM. In-capillary sample preconcentration with chemical labeling by CE offers a unique single-step analytical platform for high-throughput screening of low abundance metabolites without intrinsic chromophores. PMID:16096672

  16. Application of Doehlert designs for optimisation of an on-line preconcentration system for copper determination by flame atomic absorption spectrometry.

    PubMed

    Ferreira, Sérgio L C; Bezerra, Marcos A; Dos Santos, Walter N L; Neto, Benı X0301 Cio B

    2003-11-01

    In the present paper, a system for on-line preconcentration and determination of copper by flame atomic absorption spectrometry (FAAS) was developed. It was based on solid phase extraction of copper(II) ions on a minicolumn of Amberlite XAD-2 loaded with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM). The optimisation process was carried out using Doehlert designs. Four variables (sampling flow rate, SR; elution flow rate, buffer concentration, BC; and pH) were regarded as factors in the optimisation. The parameter "sensitivity efficiency (SE)" proposed in this paper, and defined as the analytical signal obtained for an on-line enrichment system for a preconcentration time of 1 min was used as analytical response in the optimisation process. Using the established experimental conditions, the proposed on-line system allowed determination of copper with detection limit (3sigma/S) of 0.23 mug l(-1), and a precision (repeatability), calculated as relative standard deviation (R.S.D.) of 3.9 and 3.7% for copper concentration of 5.00 and 20.00 mug l(-1), respectively. The preconcentration factor obtained is 62. The recovery achieved for copper determination in presence of several cations demonstrated that this has enough selectivity for analysis of food samples. The robustness of the proposed system was also evaluated. The accuracy was confirmed by analysis of the following certified reference materials (CRMs): Rice flour NIES 10a, Spinach leaves NIST 1570a, Apples leaves NIST 1515 and Orchard leaves NBS 1571. This procedure was applied for copper determination in natural food samples. PMID:18969189

  17. Use of factorial design and Doehlert matrix for multivariate optimisation of an on-line preconcentration system for lead determination by flame atomic absorption spectrometry.

    PubMed

    Ferreira, S L C; dos Santos, W N L; Bezerra, M A; Lemos, V A; Bosque-Sendra, J M

    2003-02-01

    A system for on-line preconcentration and determination of lead by flame atomic absorption spectrometry (FAAS) was proposed. It was based on the sorption of lead(II) ions on a minicolumn of polyurethane foam loaded with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM). The optimisation step was carried out using two-level full factorial and Doehlert designs for the determination of the optimum conditions for lead preconcentration. The proposed procedure allowed the determination of lead with a detection limit of 2.2 microg L(-1), and a precision, calculated as relative standard deviation (RSD), of 2.4 and 6.8 for a lead concentration of 50.0 and 10.0 microg L(-1), respectively. A preconcentration factor of 45 and a sampling frequency of 27 samples per hour were obtained. The recovery achieved for lead determination in the presence of several cations demonstrated that this procedure has enough selectivity for analysis of environmental samples. The validation was carried out by analysis of certified reference material. This procedure was applied to lead determination in natural food. PMID:12589511

  18. On-line preconcentration/determination of zinc from water, biological and food samples using synthesized chelating resin and flame atomic absorption spectrometry.

    PubMed

    Yılmaz, Sibel; Tokalıoğlu, Serife; Sahan, Serkan; Ulgen, Ahmet; Sahan, Ahmet; Soykan, Cengiz

    2013-04-01

    An on-line flow injection pre-concentration-flame atomic absorption spectrometry method was developed to determine trace zinc in water (tap, dam, and well water), biological (hair and nail), and liver samples. As a solid phase extractant, a synthesized new chelating resin, poly(2-thiozylmethacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propane sulfonic acid) was used. The resin was characterized by Fourier transform infrared spectroscopy, elemental analysis, and surface area by nitrogen sorption. A pre-concentration factor of 40-fold for a sample volume of 12.6 mL was obtained by using the time-based technique. The detection limit for the pre-concentration method was found to be 2.2 μg L(-1). The precision (as RSD,%) for 10 replicate determinations at the 0.04 μg mL(-1) Zn concentration was 1.2%. The calibration graph using the pre-concentration system for zinc was linear with a correlation coefficient of 0.998 in the concentration range from 0.005 to 0.05 μg mL(-1). The applicability and accuracy of the developed method were estimated by the analysis spiked water, biological, liver samples (83-105%), and also certified reference material TMDA-70 (fortified lake water) and SPS-WW1 Batch 111-Wastewater. The results were in agreement with the certified values.

  19. Determination of Hg(II) in waters by on-line preconcentration using Cyanex 923 as a sorbent — Cold vapor atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Duan, Taicheng; Song, Xuejie; Xu, Jingwei; Guo, Pengran; Chen, Hangting; Li, Hongfei

    2006-09-01

    Using a solid phase extraction mini-column home-made from a neutral extractant Cyanex 923, inorganic Hg could be on-line preconcentrated and simultaneously separated from methyl mercury. The preconcentrated Hg (II) was then eluted with 10% HNO 3 and subsequently reduced by NaBH 4 to form Hg vapor before determination by cold vapor atomic absorption spectrometry (CVAAS). Optimal conditions for and interferences on the Hg preconcentration and measurement were at 1% HCl, for a 25 mL sample uptake volume and a 10 mL min - 1 sample loading rate. The detection limit was 0.2 ng L - 1 and much lower than that of conventional method (around 15.8 ng L - 1 ). The relative standard deviation (RSD) is 1.8% for measurements of 40 ng L - 1 of Hg and the linear working curve is from 20 to 2000 ng L - 1 (with a correlation coefficient of 0.9996). The method was applied in determination of inorganic Hg in city lake and deep well water (from Changchun, Jilin, China), and recovery test results for both samples were satisfactory.

  20. On-line precipitation/dissolution system for the preconcentration and determination of manganese traces by atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Dittfurth, Carola; Ballesteros, Evaristo; Gallego, Mercedes; Valcárcel, Miguel

    1996-12-01

    Flame atomic absorption spectrometry was used for the determination of Mn in biological material following preconcentration by precipitation. The proposed preconcentration method is based on the continuous precipitation of Mn(II) as hydrated Mn(IV) oxide in ammonia buffer and dissolution of the precipitate with hydrogen oxalate or dilute nitric acid. The sensitivity of the Mn determination is increased by the presence of hydrogen peroxide, which raises the rate of oxidation of Mn(II) to Mn(IV). By using a time-based technique (at a sample loading rate of 4 ml min -1) a concentration factor of up to 55 was obtained using 24 ml of sample. The effect of concurrent cations was investigated; the most adverse effect was exerted by Fe(III), which interfered at concentrations 50 times higher than that of Mn(II).

  1. Non-chromatographic speciation analysis of mercury by flow injection on-line preconcentration in combination with chemical vapor generation atomic fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Wu, Hong; Jin, Yan; Han, Weiying; Miao, Qiang; Bi, Shuping

    2006-07-01

    A novel non-chromatographic approach for direct speciation of mercury, based on the selective retention inorganic mercury and methylmercury on the inner wall of a knotted reactor by using ammonium diethyl dithiophosphate and dithizone as complexing agents respectively, was developed for flow injection on-line sorption preconcentration coupled with chemical vapor generation non-dispersive atomic fluorescence spectrometry. With the sample pH kept at 2.0, the preconcentration of inorganic mercury on the inner walls of the knotted reactor was carried out based on the exclusive retention of Hg-DDP complex in the presence of methylmercury via on-line merging the sample solution with ammonium diethyl dithiophosphate solution, and selective preconcentration methylmercury was achieved with dithizone instead of ammonium diethyl dithiophosphate. A 15% (v/v) HCl was introduced to elute the retained mercury species and merge with KBH 4 solution for atomic fluorescence spectrometry detection. Under the optimal experimental conditions, the sample throughputs of inorganic mercury and methylmercury were 30 and 20 h - 1 with the enhancement factors of 13 and 24. The detection limits were found to be 3.6 ng l - 1 for Hg 2+ and 2.0 ng l - 1 for CH 3Hg +. The precisions (RSD) for the 11 replicate measurements of each 0.2 μg l - 1 of Hg 2+ and CH 3Hg + were 2.2% and 2.8%, respectively. The developed method was validated by the analysis of certified reference materials (simulated natural water, rice flour and pork) and by recovery measurements on spiked samples, and was applied to the determination of inorganic mercury and methylmercury in biological and environmental water samples.

  2. On-line sample preconcentration with chemical derivatization of bacterial biomarkers by capillary electrophoresis: a dual strategy for integrating sample pretreatment with chemical analysis.

    PubMed

    Ptolemy, Adam S; Le Bihan, Marianne; Britz-McKibbin, Philip

    2005-11-01

    Simple, selective yet sensitive methods to quantify low-abundance bacterial biomarkers derived from complex samples are required in clinical, biological, and environmental applications. In this report, a new strategy to integrate sample pretreatment with chemical analysis is investigated using on-line preconcentration with chemical derivatization by CE and UV detection. Single-step enantioselective analysis of muramic acid (MA) and diaminopimelic acid (DAP) was achieved by CE via sample enrichment by dynamic pH junction with ortho-phthalaldehyde/N-acetyl-L-cysteine labeling directly in-capillary. The optimized method resulted in up to a 100-fold enhancement in concentration sensitivity compared to conventional off-line derivatization procedures. The method was also applied toward the detection of micromolar levels of MA and DAP excreted in the extracellular medium of Escherichia coli bacterial cell cultures. On-line preconcentration with chemical derivatization by CE represents a unique approach for conducting rapid, sensitive, and high-throughput analyses of other classes of amino acid and amino sugar metabolites with reduced sample handling, where the capillary functions simultaneously as a concentrator, microreactor, and chiral selector.

  3. On-line sample preconcentration with chemical derivatization of bacterial biomarkers by capillary electrophoresis: a dual strategy for integrating sample pretreatment with chemical analysis.

    PubMed

    Ptolemy, Adam S; Le Bihan, Marianne; Britz-McKibbin, Philip

    2005-11-01

    Simple, selective yet sensitive methods to quantify low-abundance bacterial biomarkers derived from complex samples are required in clinical, biological, and environmental applications. In this report, a new strategy to integrate sample pretreatment with chemical analysis is investigated using on-line preconcentration with chemical derivatization by CE and UV detection. Single-step enantioselective analysis of muramic acid (MA) and diaminopimelic acid (DAP) was achieved by CE via sample enrichment by dynamic pH junction with ortho-phthalaldehyde/N-acetyl-L-cysteine labeling directly in-capillary. The optimized method resulted in up to a 100-fold enhancement in concentration sensitivity compared to conventional off-line derivatization procedures. The method was also applied toward the detection of micromolar levels of MA and DAP excreted in the extracellular medium of Escherichia coli bacterial cell cultures. On-line preconcentration with chemical derivatization by CE represents a unique approach for conducting rapid, sensitive, and high-throughput analyses of other classes of amino acid and amino sugar metabolites with reduced sample handling, where the capillary functions simultaneously as a concentrator, microreactor, and chiral selector. PMID:16200529

  4. Use of 8-hydroxyquinoline-chitosan chelating resin in an automated on-line preconcentration system for determination of zinc(II) by F AAS.

    PubMed

    Carletto, Jeferson Schneider; Roux, Kalya Cravo Di Pietro; Maltez, Heloisa França; Martendal, Edmar; Carasek, Eduardo

    2008-08-30

    This study presents the development of an on-line preconcentration system for zinc(II) determination in aqueous samples. The analyte was trapped in a mini-column filled with a chelating resin based on a chitosan biopolymer modified with 8-hydroxyquinoline obtained by the diazotization reaction. Flow and chemical variables of the system, as well as the potential interference ions, were optimized through a multivariate procedure. The factors selected were sample pH, eluent concentration (HNO(3)), and sample and eluent flow rates. It was verified through a full factorial design that the sample pH and eluent flow rate factors were statistically significant at the 95% confidence level. A final optimization of the significant factors was carried out using a Doehlert matrix. The preconcentration system was linear between 2.5 and 75 microgL(-1), with a regression coefficient of 0.9995. The enrichment factor was 17.6. The limits of detection and quantification were 0.8 and 2.5 microgL(-1), respectively. The repeatability and the analytical frequency were, respectively, 2.7 (25.0 microgL(-1), n=8) and 18 samples per hour. Results for recovery tests using mineral water samples were between 85 and 93%. Certified reference materials were analyzed in order to check the accuracy of the proposed method.

  5. Determination of benzoylureas in ground water samples by fully automated on-line pre-concentration and liquid chromatography-fluorescence detection.

    PubMed

    Gil García, M D; Martínez Galera, M; Barranco Martínez, D; Gisbert Gallego, J

    2006-01-27

    An on-line pre-concentration method for the analysis of five benzoylureas (diflubenzuron, triflumuron, hexaflumuron, lufenuron and flufenoxuron) in ground water samples was evaluated using two C(18) columns, and fluorescence detection after photochemical induced fluorescence (PIF) post-column derivatization. The trace enrichment was carried out with 35 mL of ground water modified with 15 mL of MeOH on a 50 mm x 4.6 mm I.D. first enrichment column (C-1) packed with 5 microm Hypersil Elite C(18). Retention properties of pesticides and humic acids usually contained in ground water were studied on C-1 at concentration levels ranging between 0.04 and 14.00 microg/L in water samples. The results obtained in this study show that the pesticides are pre-concentrated in the first short column while the humic acids contained in the ground water samples are eluted to waste. Pesticides recoveries ranged between 92.3 and 109.5%. The methodology proposed was used to determine benzoylureas in ground water samples at levels lower than 0.1 microg/L (maximum levels established by the European Union). PMID:16337641

  6. Automated on-line preconcentration of trace aqueous mercury with gold trap focusing for cold vapor atomic absorption spectrometry.

    PubMed

    Puanngam, Mahitti; Dasgupta, Purnendu K; Unob, Fuangfa

    2012-09-15

    A fully automated system for the determination of trace mercury in water by cold vapor atomic absorption spectrometry (CVAAS) is reported. The system uses preconcentration on a novel sorbent followed by liberation of the mercury and focusing by a gold trap. Mercury ions were extracted from water samples by passage through a solid phase sorbent column containing 2-(3-(2-aminoethylthio)propylthio)ethanamine modified silica gel. The captured mercury is released by thiourea and then elemental Hg is liberated by sodium borohydride. The vapor phase Hg is recaptured on a gold-plated tungsten filament. This is liberated as a sharp pulse (half-width<2 s) by directly electrically heating the tungsten filament in a dry argon stream. The mercury is measured by CVAAS; no moisture removal is needed. The effects of chloride and selected interfering ions were studied. The sample loading flow rate and argon flow rates for solution purging and filament sweeping were optimized. An overall 50-fold improvement in the limit of detection was observed relative to direct measurement by CVAAS. With a relatively modest multi-user instrument we attained a limit of detection of 35 ng L(-1) with 12% RSD at 0.20 μg L(-1) Hg level. The method was successfully applied to accurately determine sub-μg L(-1) level Hg in standard reference water samples.

  7. Application of multiwall carbon nanotubes impregnated with 5-dodecylsalicylaldoxime for on-line copper preconcentration and determination in water samples by flame atomic absorption spectrometry.

    PubMed

    Tobiasz, Anna; Walas, Stanisław; Soto Hernández, Arlene; Mrowiec, Halina

    2012-07-15

    The paper presents application of multiwall carbon nanotubes (MWCNTs) modified with 5-dodecylsalicylaldoxime to copper(II) flow-injection on-line preconcentration and flame atomic absorption spectrometric (FAAS) determination. Two new sorbents were obtained by impregnation of MWCNTs with Cu(II)-LIX 622(®) complex, however in the first case modification was preceded by carbon wall activation via oxidization (Cu-LIX-CNT-A sorbent), and in the second one no surface activation was performed (Cu-LIX-CNT sorbent). It was found that effective leaching of initially introduced copper and Cu(II) retained in preconcentration process could be realized with the use 7% and 5% (v/v) nitric acid, for particular sorbents. Testing the influence of loading solution pH and rate of loading on sorption it was found out that optimal range of loading solution pH was about 4.5-6.3 for activated and 6.15-6.25 for non-activated CNT. Investigation of sorption kinetics showed that the process can be described by pseudo-second order reaction model. Sorption equilibrium conditions (90% sorption) for LIX-CNT-A and LIX-CNT were obtained after 8-15min, respectively and maximum sorption capacity for the new sorbents amounted to 18.1mgg(-1) and 31.6mgg(-1), respectively. For the examined sorbents enrichment factors increased with extension of loading time up to 180s: linearly for activated and non-linearly for non-activated MWCNTs. Influence of potential interferents such as Cd(II), Zn(II), Fe(III), Mg(II) and Ca(II) ions on copper(II) sorption on the new CNT materials was examined individually and with the use of 2(5-2) factorial design. The study revealed significant interference from iron, magnesium and calcium ions at relatively high concentrations. Applicability of the proposed sorbents was tested for Cu(II) determination in various kinds of water samples and the results were compared with those obtained with the use of ICP MS as a reference technique. Copper(II) determination in two certified

  8. Determination of carbofuran in surface water and biological tissue by sol-gel immunoaffinity extraction and on-line preconcentration/HPLC/UV analysis.

    PubMed

    Vera-Avila, Luz E; Márquez-Lira, Bani P; Villanueva, Marcos; Covarrubias, Rosario; Zelada, Gustavo; Thibert, Valérie

    2012-01-15

    A selective and simple analytical method for the trace level determination of carbofuran in complex environmental and biological samples was developed based on immunoaffinity extraction (IAE) followed by on-line preconcentration and HPLC/UV analysis of the purified extract. The immunosorbent for IAE was prepared by sol-gel encapsulation of monoclonal anti-carbofuran antibodies, and was fully characterized for capacity, repeatability, binding strength, binding kinetics and cross-reactivity. Method performance was evaluated with two different types of difficult samples: dam water and methanolic extracts of epithelial cervical-uterine tissue. Linear behavior and quantitative recoveries were obtained from the analysis of samples spiked with carbofuran at 0.2-4 ng/mL (dam water, 50 mL samples) and 10-40 ng/mL (biological tissue extract, 2 mL samples). RSD (n=7) and detection limits were, respectively, 10.1% (spike 0.40 ng/mL) and 0.13 ng/mL for dam water; 8.5% (spike 20 ng/mL) and 5 ng/mL for the biological tissue extract. The excellent sample purification achieved with the IAE column allows precise and accurate determination of carbofuran in complex matrices, even when using non-selective UV detection in the chromatographic analysis.

  9. Simultaneous determination of nanomole amounts of sulphur dioxide and hydrogen sulphide by flow injection analysis with on-line preconcentration by means of capillary denuder tubes.

    PubMed

    Achilli, Marco; Gács, Istvan

    2002-01-01

    A simple and rapid method for trace determination of SO2 and H2S in gaseous samples by using a flow injection system with on line preconcentration on capillary denuder is described. The gaseous samples are led through a 0.4 M sulphamic acid solution, retaining nitrogen dioxide, ammonia and hydrogen chloride. The sulphur dioxide is collected from the carrier gas stream (250 cm3 min-1) as sulphuric acid in a capillary denuder tube coated with a thin layer of 0.01-0.03 M hydrogen peroxide solution of 0.05 mM sulphuric acid; hydrogen sulphide passes into a second tube coated with 0.075 mM sodium sulphide solution of 0.1 M aqueous sodium hydroxide. The films containing the sulphuric acid and the sodium sulphide, respectively, are eluted with the corresponding circulating absorbent streams and pass through the detectors. Sulphuric acid is detected by conductimetry and sulphide is determined spectrophotometrically at 230 nm. If nanoequivalent amounts of H2S are present in the sample containing a large concentration of SO2 (SO2/H2S concentration ratio > 20), the sulphur dioxide is filtered out of the sample gas stream by solid sodium hydrogen carbonate. A limit of detection of 3.5 micrograms m-3 is obtained.

  10. High-sensitivity capillary electrophoresis determination of inorganic anions in serum and urine using on-line preconcentration by transient isotachophoresis.

    PubMed

    Hirokawa, Takeshi; Yoshioka, Masato; Okamoto, Hikaru; Timerbaev, Andrei R; Blaschke, Gottfried

    2004-11-25

    Concentrations of inorganic anions, both as individual species and biotransformation products, in physiological fluids are of strong concern in clinical studies. To date, analytical methodologies have either required different analytical procedures to determine these analytes in plasma and urine, or extensive sample preparation, or unconventional and often expensive detection schemes, or both. A simple and sensitive capillary electrophoresis (CE) method with direct UV detection was developed for the simultaneous determination of iodide, bromide and nitrate in human plasma and urine, with a special focus on reliable quantification of the trace serum iodide. With the latter objective, the method incorporates a transient isotachophoresis (tITP) procedure enabling an efficient on-line preconcentration of iodide (limit of detection, 1.4 microg l(-1)) as well as other moderately mobile analytes that fall into the tITP range. The analyses of both types of biofluids were performed using an acidic electrolyte system composed of 0.25 mol l(-1) sodium chloride and 7.5 mmol l(-1) cetyltrimethylammonium chloride at pH 2.2 and 0.5 mol l(-1) 2-(N-morpholino)ethanesulfonate (pH 6.0) as terminating electrolyte. Relative standard deviations (R.S.D.) below 3.0% and 9.2% were obtained for within-day and between-day precision, respectively. Resolution and quantification of oxalic acid was also feasible under optimized tITP-CE conditions. Sample preparation required only ultrafiltration (serum) and dilution (urine). A number of plasma and urine samples were evaluated with this assay and the iodide, bromide and nitrate concentrations were in the expected clinical concentration ranges. PMID:15522716

  11. Determination of trace metals in urine with an on-line ultrasound-assisted digestion system combined with a flow-injection preconcentration manifold coupled to flame atomic absorption spectrometry.

    PubMed

    Cespón-Romero, R M; Yebra-Biurrun, M C

    2008-02-25

    A flow analysis method with on-line sample digestion/minicolumn preconcentration/flame atomic absorption spectrometry is described for the determination of trace metals in urine. First, urine sample was on-line ultrasound-assisted digested exploiting the stopped-flow mode, and then the metals were preconcentrated passing the pre-treated sample through a minicolumn containing a chelating resin. A home-made minicolumn of commercially available imminodiacetic functional group resin, Chelite Che was used to preconcentrate trace metals (Cu, Fe, Mn and Ni) from urine. The proposed procedure allowed the determination of the metals with detection limits of 0.5, 1.1, 0.8 and 0.8microgL(-1), for Cu, Fe, Mn and Ni, respectively. The precision based on replicate analysis was less than +/-10.0%, and the enrichment factor obtained was between 21.3 (Mn) and 44.1 (Ni), for sample volumes between 2.5 and 5.0mL, and an eluent volume of 110microL. This procedure was applied for determination of metals in urine of workers exposed to welding fumes and urine of unexposed persons (urine control).

  12. On-line preconcentration and determination of copper, lead and chromium(VI) using unloaded polyurethane foam packed column by flame atomic absorption spectrometry in natural waters and biological samples.

    PubMed

    Anthemidis, Aristidis N; Zachariadis, George A; Stratis, John A

    2002-11-12

    A simple, sensitive and low cost, flow injection time-based method was developed for on-line preconcentration and determination of copper, lead and chromium(VI) at sub mug l(-1) levels in natural waters and biological samples. At the optimum pH, the on-line formed metal-ammonium pyrrolidine dithiocarbamate (APDC) complexes were sorbed on the unloaded commercial polyurethane foam (PUF), and subsequent eluted quantitatively by isobutylmethylketone and determined by flame atomic absorption spectrometry (FAAS). All chemical, and flow injection variables were optimized for the quantitative preconcentration of each metal and a study of interference level of various ions was also carried out. The system offered improved flexibility, low backpressure and applicability to all the studied metals. At a sample frequency of 36 h(-1) and a 60 s preconcentration time, the enhancement factor was 170, 131 and 28, the detection limit was 0.2, 1.8 and 2.0 mug l(-1), and the precision, expressed as relative standard deviation (s(r)), was 2.8 (at 10 mug l(-1)), 3.4 (at 50 mug l(-1)) and 3.6% (at 50 mug l(-1)) for Cu(II), Pb(II) and Cr(VI), respectively. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference materials and spiked water samples. Finally, the method was applied to the analysis of environmental samples. PMID:18968813

  13. Preliminary results on the determination of ultratrace amounts of cadmium in tea samples using a flow injection on-line solid phase extraction separation and preconcentration technique to couple with a sequential injection hydride generation atomic fluorescence spectrometry.

    PubMed

    Duan, Taicheng; Song, Xuejie; Jin, Dan; Li, Hongfei; Xu, Jingwei; Chen, Hangting

    2005-10-31

    In this work, a method was developed for determination of ultra-trace levels of Cd in tea samples by atomic fluorescence spectrometry (AFS). A flow injection solid phase extraction (FI-SPE) separation and preconcentration technique, to on-line couple with a sequential injection hydride generation (SI-HG) technique is employed in this study. Cd was preconcentrated on the SPE column, which was made from a neutral extractant named Cyanex 923, while other matrix ions or interfering ions were completely or mostly separated off. Conditions for the SPE separation and preconcentration, as well as conditions for the HG technique, were studied. Due to the separation of interfering elements, Cd hydride generation efficiency could be greatly enhanced with the sole presence of Co(2+) with a concentration of 200mugL(-1), which is much lower than those in other works previously reported. Interferences on both the Cd separation and preconcentration, and Cd hydride generation (HG) were investigated; it showed that both the separation and preconcentration system, and the HG system had a strong anti-interference ability. The SPE column could be repeatedly used at least 400 times, a R.S.D. of 0.97% was obtained for 6 measurements of Cd with 0.2mugL(-1) and a correlation coefficiency of 1.0000 was obtained for the measurement of a series of solutions with Cd concentrations from 0.1 to 2mugL(-1). The method has a low detection limit of 10.8ngL(-1) for a 25mL solution and was successfully validated by using two tea standard reference materials (GBW08513 and GBW07605).

  14. Analysis of biogenic carbonates by inductively coupled plasma-mass spectrometry (ICP-MS). Flow injection on-line solid-phase preconcentration for trace element determination in fish otoliths.

    PubMed

    Arslan, Z; Paulson, A J

    2002-04-01

    The aragonite deposits within the ear bones (otoliths) of teleost fish retain a chemical signal reflecting the life history of fish (similar to rings of trees) and the nature of fish habitats. Otoliths dissolved in acid solutions contain high concentrations of calcium and a variety of proteins. Elimination of matrix salts and organic interferences during preconcentration is essential for accurate determination of trace elements in otolith solutions by inductively coupled plasma-quadrupole mass spectrometry. An iminodiacetate-based chelating resin (Toyopearl AF-Chelate 650 M) has been used for on-line preconcentration and matrix separation for the determination of 31 transition and rare elements. Successful preconcentration of the elements was achieved at pH 5 by on-line buffering, except Mn which required pH 8.8. Sample solutions were loaded on to the column for 1 min at 3.2 mL min(-1), and then eluted directly into the mass spectrometer with 4% v/v nitric acid. This procedure enabled up to 25-fold preconcentration with successful removal of the calcium matrix. The effect of heat-assisted oxidation with concentrated nitric acid was investigated to eliminate the organic matrix. It was found that heating to dryness after dissolution and further mineralization with the acid significantly improved the retention of the transition elements. The method was validated by analysis of a certified reference material produced from saggittal otoliths of emperor snapper ( Lutjanus sebae), and then applied to the determination of trace metal concentrations in juvenile bluefin tuna ( Thunnus thynnus) from the Western Pacific Ocean.

  15. Trace level determination of cadmium in wine by on-line preconcentration in a 5-Br-PADAP functionalized wool-packed microcolumn coupled to flame atomic absorption spectrometry.

    PubMed

    Monasterio, Romina P; Wuilloud, Rodolfo G

    2009-10-15

    An on-line retention and preconcentration system based on a sheep wool-packed microcolumn combined with flame atomic absorption spectrometry is proposed for trace level determination of Cd in wine. A chelating reagent 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol was immobilized onto the wool before retention of the analyte. Several factors influencing the preconcentration efficiency of Cd and his subsequent determination, such as pH, eluent type, sample and eluent flow rates, interfering effects, were studied. A preconcentration factor of 39 was obtained with only 20 mL of sample. The relative standard deviation for five determinations of 1 microg L(-1) Cd was 3.4%. The calibration graph was linear with a correlation coefficient of 0.998 at levels near the detection limit and up to at least 25 microg L(-1). The limit of detection was 37 ng L(-1). The accuracy of the proposed methodology was tested by comparison of the results with those obtained by electrothermal atomic absorption spectrometry analysis along with a recovery study. Finally, the method was employed for evaluating Cd levels in different wines including, blank, rose, and red.

  16. Adsorption studies of Cd(II) onto Al 2O 3/Nb 2O 5 mixed oxide dispersed on silica matrix and its on-line preconcentration and determination by flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mendonça Costa, Lucimara; Ribeiro, Emerson Schwingel; Segatelli, Mariana Gava; do Nascimento, Danielle Raphael; de Oliveira, Fernanda Midori; Tarley, César Ricardo Teixeira

    2011-05-01

    The present study describes the adsorption characteristic of Cd(II) onto Nb 2O 5/Al 2O 3 mixed oxide dispersed on silica matrix. The characterization of the adsorbent has been carried out by infrared spectroscopy (IR), scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), energy dispersive X-ray fluorescence analysis (EDXRF) and specific surface area ( SBET). From batch experiments, adsorption kinetic of Cd(II) was described by a pseudo-second-order kinetic model. The Langmuir linear isotherm fitted to the experimental adsorption isotherm very well, and the maximum adsorption capacity was found to be 17.88 mg g -1. Using the effective material, a method for Cd(II) preconcentration at trace level was developed. The method was based on on-line adsorption of Cd(II) onto SiO 2/Al 2O 3/Nb 2O 5 at pH 8.64, in which the quantitative desorption occurs with 1.0 mol L -1 hydrochloric acid towards FAAS detector. The experimental parameters related to the system were studied by means of multivariate analysis, using 2 4 full factorial design and Doehlert matrix. The effect of SO 42-, Cu 2+, Zn 2+ and Ni 2+ foreign ions showed no interference at 1:100 analyte:interferent proportion. Under the most favorable experimental conditions, the preconcentration system provided a preconcentration factor of 18.4 times, consumption index of 1.08 mL, sample throughput of 14 h -1, concentration efficiency of 4.35 min -1, linear range from 5.0 up to 35.0 μg L -1 and limits of detection and quantification of 0.19 and 0.65 μg L -1 respectively. The feasibility of the proposed method for Cd(II) determination was assessed by analysis of water samples, cigarette sample and certified reference materials TORT-2 (Lobster hepatopancreas) and DOLT-4 (Dogfish liver).

  17. Preparation and characterization of magnetic nanoparticles for the on-line determination of gold, palladium, and platinum in mine samples based on flow injection micro-column preconcentration coupled with graphite furnace atomic absorption spectrometry.

    PubMed

    Ye, Juanjuan; Liu, Shuxia; Tian, Miaomiao; Li, Wanjun; Hu, Bin; Zhou, Weihong; Jia, Qiong

    2014-01-01

    A simple and highly selective procedure for on-line determination of trace levels of Au, Pd, and Pt in mine samples has been developed using flow injection-column adsorption preconcentration coupled with graphite furnace atomic absorption spectrophotometry (FI-column-GFAAS). The precious metals were adsorbed on the as-synthesized magnetic nanoparticles functionalized with 4'-aminobenzo-15-crown-5-ether packed into a micro-column and then eluted with 2% thiourea + 0.1 mol L(-1) HCl solution prior to the determination by GFAAS. The properties of the magnetic adsorbents were investigated by scanning electron microscope (SEM), X-ray diffraction (XRD), and vibrating sample magnetometer (VSM). Various experimental parameters affecting the preconcentration of Au, Pd, and Pt were investigated and optimized. Under the optimal experimental conditions, the detection limits of the developed technique were 0.16 ng mL(-1) for Au, 0.28 ng mL(-1) for Pd, and 1.01 ng mL(-1) for Pt, with enrichment factors of 24.3, 13.9, and 17.8, respectively. Precisions, evaluated as repeatability of results, were 1.1%, 3.9%, and 4.4% respectively for Au, Pd, and Pt. The developed method was validated by the analysis of Au, Pd, and Pt in certified reference materials and mine samples with satisfactory results.

  18. Trace elements determination in seawater by ICP-MS with on-line pre-concentration on a Chelex-100 column using a ‘standard’ instrument setup.

    PubMed Central

    Søndergaard, Jens; Asmund, Gert; Larsen, Martin M.

    2015-01-01

    Trace element determination in seawater is analytically challenging due to the typically very low concentrations of the trace elements and the potential interference of the salt matrix. A common way to address the challenge is to pre-concentrate the trace elements on a chelating resin, then rinse the matrix elements from the resin and subsequently elute and detect the trace elements using inductively coupled plasma mass spectrometry (ICP-MS). This technique typically involves time-consuming pre-treatment of the samples for ‘off-line’ analyses or complicated sample introduction systems involving several pumps and valves for ‘on-line’ analyses. As an alternative, the following method offers a simple method for ‘on-line’ analyses of seawater by ICP-MS. As opposed to previous methods, excess seawater was pumped through the nebulizer of the ICP-MS during the pre-concentration step but the gas flow was adjusted so that the seawater was pumped out as waste without being sprayed into the instrument. Advantages of the method include: • Simple and convenient analyses of seawater requiring no changes to the ‘standard’ sample introduction system except from a resin-filled micro-column connected to the sample tube. The ‘standard’ sample introduction system refers to that used for routine digest-solution analyses of biota and sediment by ICP-MS using only one peristaltic pump; and • Accurate determination of the elements V, Mn, Co, Ni, Cu, Zn, Cd and Pb in a range of different seawater matrices verified by participation in 6 successive rounds of the international laboratory intercalibration program QUASIMEME. PMID:26258050

  19. Quantitative on-line preconcentration-liquid chromatography coupled with tandem mass spectrometry method for the determination of pharmaceutical compounds in water.

    PubMed

    Idder, Salima; Ley, Laurent; Mazellier, Patrick; Budzinski, Hélène

    2013-12-17

    One of the current environmental issues concerns the presence and fate of pharmaceuticals in water bodies as these compounds may represent a potential environmental problem. The characterization of pharmaceutical contamination requires powerful analytical method able to quantify these pollutants at very low concentration (few ng L(-1)). In this work, a multi-residue analytical methodology (on-line solid phase extraction-liquid chromatography-triple quadrupole mass spectrometry using positive and negative electrospray ionization) has been developed and validated for 40 multi-class pharmaceuticals and metabolites for tap and surface waters. This on-line SPE method was very convenient and efficient compared to classical off-line SPE method because of its shorter total run time including sample preparation and smaller sample volume (1 mL vs up to 1 L). The optimized method included several therapeutic classes as lipid regulators, antibiotics, beta-blockers, non-steroidal anti-inflammatories, antineoplastic, etc., with various physicochemical properties. Quantification has been achieved with the internal standards. The limits of detection are between 0.7 and 15 ng L(-1) for drinking waters and 2-15 ng L(-1) for surface waters. The inter-day precision values are below 20% for each studied level. The improvement and strength of the analytical method has been verified along a monitoring of these 40 pharmaceuticals in Isle River, a French stream located in the South West of France. During this survey, 16 pharmaceutical compounds have been detected.

  20. Modified mesoporous silica materials for on-line separation and preconcentration of hexavalent chromium using a microcolumn coupled with flame atomic absorption spectrometry.

    PubMed

    Wang, Zheng; Fang, Dong-Mei; Li, Qing; Zhang, Ling-Xia; Qian, Rong; Zhu, Yan; Qu, Hai-Yun; Du, Yi-Ping

    2012-05-01

    A modified SBA-15 mesoporous silica material NH(2)-SBA-15 was synthesized successfully by grafting γ-aminopropyl-triethoxysilane. The material was characterized using transmission electron microscopy (TEM) and Fourier transform infrared/Raman (FT-IR/Raman) spectroscopy, and used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Effective sorption of Cr (VI) was achieved at pH 2.0 with no interference from Cr (III) and other ions and 0.5 mol L(-1) NH(3)·H(2)O solution was found optimal for the complete elution of Cr (VI). An enrichment factor of 44 and was achieved under optimized experimental conditions at a sample loading of 2.0 mL min(-1) sample loading (300 s) and an elution flow rate of 2.0 mL min(-1) (24s). The precision of the 11 replicate Cr (VI) measurements was 2.1% at the 100 μg L(-1) level with a detection limit of 0.2 μg L(-1) (3s, n=10) using the FAAS. The developed method was successfully applied to trace chromium determination in waste water. The accuracy was validated using a certified reference material of riverine water (GBW08607). PMID:22502615

  1. On-line analysis of volatile chlorinated hydrocarbons in air by gas chromatography-mass spectrometry Improvements in preconcentration and injection steps.

    PubMed

    Zoccolillo, Lelio; Amendola, Luca; Insogna, Susanna; Pastorini, Elisabetta

    2010-06-11

    An analytical system composed of a cryofocusing trap injector device coupled to a gas chromatograph with mass spectrometric detection (CTI-GC-MS) specific for the on-line analysis in air of volatile chlorinated hydrocarbons (VCHCs) (dichloromethane; chloroform; 1,1,1-trichloroethane; tetrachloromethane; 1,1,2-trichloroethylene; tetrachloroethylene) was developed. The cryofocusing trap injector was the result of appropriate low cost modifications to an original purge-and-trap device to make it suitable for direct air analysis even in the case of only slightly contaminated air samples, such as those from remote zones. The CTI device can rapidly and easily be rearranged into the purge-and-trap allowing water and air analysis with the same apparatus. Air samples, collected in stainless steel canisters, were introduced directly into the CTI-GC-MS system to realize cryo-concentration (at -120 degrees C), thermal desorption (at 200 degrees C) and for the subsequent analysis of volatiles. The operating phases and conditions were customised and optimized. Recovery efficiency was optimized in terms of moisture removal, cold trap temperature and sampling mass flow. The injection of entrapped volatiles was realized through a direct transfer with high chromatographic reliability (capillary column-capillary column). These improvements allowed obtaining limits of detection (LODs) at least one order of magnitude lower than current LODs for the investigated substances. The method was successfully employed on real samples: air from urban and rural areas and air from remote zones such as Antarctica.

  2. Determination of rare earth elements in seawater by inductively coupled plasma mass spectrometry with on-line column pre-concentration using 8-quinolinole-immobilized fluorinated metal alkoxide glass

    NASA Astrophysics Data System (ADS)

    Kajiya, Tasuku; Aihara, Masato; Hirata, Shizuko

    2004-04-01

    The on-line column pre-concentration technique with inductively coupled plasma mass spectrometry (ICP-MS) has been developed using micro-column of 8-quinolinole-immobilized fluorinated metal alkoxide glass (MAF-8HQ). The aim of method was to determine rare earth elements (REEs) (Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in seawater. A 6.4 ml of seawater sample was passed through the column for 2 min, after washing the column with ultrapure water, the adsorbed REEs were subsequently eluted into the plasma with 1.4 M nitric acid. Sample pH, sampling and eluting flow rates and acidity of eluent were optimized. Detection limits (3 σ) based on three times standard deviations of water by 8 replicates were in the range from 0.11 pg ml -1 for Y to 0.30 pg ml -1 for Tb, and the precisions by a 10 pg ml -1 REEs standard solution ( n=8) were in the range from 4.7% for Tm to 8.7% for Tb and Yb. Analysis of one sample could be processed in 7 min. The proposed method was verified by determination of REEs in the two certified reference materials (CRMs) of seawater, CASS-4 and NASS-5, and the method was also applied to determine REEs in the costal seawater of Hiroshima Bay, the Seto Inland Sea, Japan.

  3. Determination of (ultra)trace amounts of arsenic(III) and arsenic(V) in water by inductively coupled plasma mass spectrometry coupled with flow injection on-line sorption preconcentration and separation in a knotted reactor.

    PubMed

    Yan, X P; Kerrich, R; Hendry, M J

    1998-11-15

    A method has been developed for determination of (ultra)trace amounts of As(III) and As(V) in water by flow injection on-line sorption preconcentration and separation coupled with inductively coupled plasma mass spectrometry (ICPMS) using a knotted reactor (KR). The determination of As(III) was achieved by selective formation of the As(III)-pyrrolidine dithiocarbamate complex over a sample acidity range of 0.01-0.7 mol L-1 HNO3, its adsorption onto the inner walls of the KR made from 150-cm-long, 0.5-mm-i.d. PTFE tubing, elution with 1 mol L-1 HNO3, and detection by ICPMS. Total inorganic arsenic was determined after prereduction of As(V) to As(III) in a 1% (m/v) L-cysteine-0.03 mol L-1 HNO3 media. The concentration of As(V) was calculated by difference (the total inorganic arsenic and As(III)). Owing to the group-specific character of the chelating agent, and the use of an efficient rinsing step before elution, the interferences encountered in conventional ICPMS from common major matrix, alkali and alkaline earth metals, and chlorides were eliminated. The presence of organoarsenic species such as monomethylarsonate and dimethylarsinate in water samples had no effect on the results of As(III) and As(V). Thus, the method can be applied to the speciation analysis of inorganic arsenic at submicrogram per liter levels in aqueous solutions with high total content of dissolved solid and/or high content of chlorides. Using a preconcentration time of 60 s and a sample flow rate of 5 mL min-1, an enhancement factor of 22 was achieved in comparison with conventional ICPMS. The time required for a single determination was 200 s. The detection limits (3s) was evaluated to be 0.021 microgram L-1 for As(III) and 0.029 microgram L-1 for total inorganic arsenic. The precision for 14 replicate determinations of 1 microgram L-1 As(III) was 2.8% (RSD) with drift correction and 3.9% (RSD) without drift correction. The concentrations of As(III) and As(V) in synthetic mixtures obtained

  4. Biological preconcentrator

    DOEpatents

    Manginell, Ronald P.; Bunker, Bruce C.; Huber, Dale L.

    2008-09-09

    A biological preconcentrator comprises a stimulus-responsive active film on a stimulus-producing microfabricated platform. The active film can comprise a thermally switchable polymer film that can be used to selectively absorb and desorb proteins from a protein mixture. The biological microfabricated platform can comprise a thin membrane suspended on a substrate with an integral resistive heater and/or thermoelectric cooler for thermal switching of the active polymer film disposed on the membrane. The active polymer film can comprise hydrogel-like polymers, such as poly(ethylene oxide) or poly(n-isopropylacrylamide), that are tethered to the membrane. The biological preconcentrator can be fabricated with semiconductor materials and technologies.

  5. Sequential injection-bead injection-lab-on-valve coupled to high-performance liquid chromatography for online renewable micro-solid-phase extraction of carbamate residues in food and environmental samples.

    PubMed

    Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax; Grudpan, Kate

    2011-07-01

    A sequential injection-bead injection-lab-on-valve system was hyphenated to HPLC for online renewable micro-solid-phase extraction of carbamate insecticides. The carbamates studied were isoprocarb, methomyl, carbaryl, carbofuran, methiocarb, promecarb, and propoxur. LiChroprep(®) RP-18 beads (25-40 μm) were employed as renewable sorbent packing in a microcolumn situated inside the LOV platform mounted above the multiposition valve of the sequential injection system. The analytes sorbed by the microcolumn were eluted using 80% acetonitrile in 0.1% acetic acid before online introduction to the HPLC system. Separation was performed on an Atlantis C-18 column (4.6 × 150 mm, 5 μm) utilizing gradient elution with a flow rate of 1.0 mL/min and a detection wavelength at 270 nm. The sequential injection system offers the means of performing automated handling of sample preconcentration and matrix removal. The enrichment factors ranged between 20 and 125, leading to limits of detection (LODs) in the range of 1-20 μg/L. Good reproducibility was obtained with relative standard deviations of <0.7 and 5.4% for retention time and peak area, respectively. The developed method has been successfully applied to the determination of carbamate residues in fruit, vegetable, and water samples.

  6. Particle preconcentrator

    SciTech Connect

    Linker, K.L.; Conrad, F.J.; Custer, C.A.; Rhykerd, C.L. Jr

    2000-07-11

    An apparatus and method are disclosed for preconcentrating particles and vapors. The preconcentrator apparatus permits detection of highly diluted amounts of particles in a main gas stream, such as a stream of ambient air. A main gas stream having airborne particles entrained therein is passed through a previous screen. The particles accumulate upon the screen, as the screen acts as a sort of selective particle filter. The flow of the main gas stream is then interrupted by diaphragm shutter valves, whereupon a cross-flow of carrier gas stream is blown parallel past the faces of the screen to dislodge the accumulated particles and carry them to a particle or vapor detector, such as an ion mobility spectrometer. The screen may be heated, such as by passing an electrical current there through, to promote desorption of particles therefrom during the flow of the carrier gas. Various types of screens are disclosed. The apparatus and method of the invention may find particular utility in the fields of narcotics, explosives detection and chemical agents.

  7. Chemical preconcentrator

    DOEpatents

    Manginell, Ronald P.; Frye-Mason, Gregory C.

    2001-01-01

    A chemical preconcentrator is disclosed with applications to chemical sensing and analysis. The preconcentrator can be formed by depositing a resistive heating element (e.g. platinum) over a membrane (e.g. silicon nitride) suspended above a substrate. A coating of a sorptive material (e.g. a microporous hydrophobic sol-gel coating or a polymer coating) is formed on the suspended membrane proximate to the heating element to selective sorb one or more chemical species of interest over a time period, thereby concentrating the chemical species in the sorptive material. Upon heating the sorptive material with the resistive heating element, the sorbed chemical species are released for detection and analysis in a relatively high concentration and over a relatively short time period. The sorptive material can be made to selectively sorb particular chemical species of interest while not substantially sorbing other chemical species not of interest. The present invention has applications for use in forming high-sensitivity, rapid-response miniaturized chemical analysis systems (e.g. a "chem lab on a chip").

  8. Particle preconcentrator

    DOEpatents

    Linker, Kevin L.; Conrad, Frank J.; Custer, Chad A.; Rhykerd, Jr., Charles L.

    1998-01-01

    An apparatus and method for preconcentrating particles and vapors. The preconcentrator apparatus permits detection of highly diluted amounts of particles in a main gas stream, such as a stream of ambient air. A main gas stream having airborne particles entrained therein is passed through a pervious screen. The particles accumulate upon the screen, as the screen acts as a sort of selective particle filter. The flow of the main gas stream is then interrupted by diaphragm shutter valves, whereupon a cross-flow of carrier gas stream is blown parallel past the faces of the screen to dislodge the accumulated particles and carry them to a particle or vapor detector, such as an ion mobility spectrometer. The screen may be heated, such as by passing an electrical current there through, to promote desorption of particles therefrom during the flow of the carrier gas. Various types of screens are disclosed. The apparatus and method of the invention may find particular utility in the fields of narcotics, explosives detection and chemical agents.

  9. Particle preconcentrator

    DOEpatents

    Linker, Kevin L.; Conrad, Frank J.; Custer, Chad A.; Rhykerd, Jr., Charles L.

    2000-01-01

    An apparatus and method for preconcentrating particles and vapors. The preconcentrator apparatus permits detection of highly diluted amounts of particles in a main gas stream, such as a stream of ambient air. A main gas stream having airborne particles entrained therein is passed through a pervious screen. The particles accumulate upon the screen, as the screen acts as a sort of selective particle filter. The flow of the main gas stream is then interrupted by diaphragm shutter valves, whereupon a cross-flow of carrier gas stream is blown parallel past the faces of the screen to dislodge the accumulated particles and carry them to a particle or vapor detector, such as an ion mobility spectrometer. The screen may be heated, such as by passing an electrical current there through, to promote desorption of particles therefrom during the flow of the carrier gas. Various types of screens are disclosed. The apparatus and method of the invention may find particular utility in the fields of narcotics, explosives detection and chemical agents.

  10. Particle preconcentrator

    DOEpatents

    Linker, Kevin L.; Conrad, Frank J.; Custer, Chad A.; Rhykerd, Jr., Charles L.

    2005-09-20

    An apparatus and method for preconcentrating particles and vapors. The preconcentrator apparatus permits detection of highly diluted amounts of particles in a main gas stream, such as a stream of ambient air. A main gas stream having airborne particles entrained therein is passed through a pervious screen. The particles accumulate upon the screen, as the screen acts as a sort of selective particle filter. The flow of the main gas stream is then interrupted by diaphragm shutter valves, whereupon a cross-flow of carrier gas stream is blown parallel past the faces of the screen to dislodge the accumulated particles and carry them to a particle or vapor detector, such as an ion mobility spectrometer. The screen may be heated, such as by passing an electrical current there through, to promote desorption of particles therefrom during the flow of the carrier gas. Various types of screens are disclosed. The apparatus and method of the invention may find particular utility in the fields of narcotics, explosives detection and chemical agents.

  11. Particle preconcentrator

    DOEpatents

    Linker, K.L.; Conrad, F.J.; Custer, C.A.; Rhykerd, C.L. Jr.

    1998-12-29

    An apparatus and method are disclosed for preconcentrating particles and vapors. The preconcentrator apparatus permits detection of highly diluted amounts of particles in a main gas stream, such as a stream of ambient air. A main gas stream having airborne particles entrained therein is passed through a pervious screen. The particles accumulate upon the screen, as the screen acts as a sort of selective particle filter. The flow of the main gas stream is then interrupted by diaphragm shutter valves, whereupon a cross-flow of carrier gas stream is blown parallel past the faces of the screen to dislodge the accumulated particles and carry them to a particle or vapor detector, such as an ion mobility spectrometer. The screen may be heated, such as by passing an electrical current there through, to promote desorption of particles therefrom during the flow of the carrier gas. Various types of screens are disclosed. The apparatus and method of the invention may find particular utility in the fields of narcotics, explosives detection and chemical agents. 3 figs.

  12. Exploiting the bead injection concept for sequential determination of copper and mercury ions in river-water samples.

    PubMed

    Vidotti, Eliane C; Almeida, Vitor C; Oliveira, Cláudio C

    2004-11-15

    A procedure involving bead-injection concept and sequential determination of copper and mercury ions in river-water samples is proposed. The method is based on the solid-phase extraction of both metal ions on the same beads surface (Chelex 100 resin) and in their subsequent reaction with the colorimetric reagents (APDC and Dithizone for copper and mercury ions, respectively). For this task, a resin mini-column is established in the optical path by the selection, introduction and trapping of a defined volume of the Chelex-100 resin beads suspension in the flow system. The passage of the sample solution through the resin mini-column promotes the sorption of Cu(II) ions and, making the APDC colorimetric reagent flows through the beads, the formation of the coloured complex on the solid phase surface occurs. The absorbance of the formed APDC-Cu complex is then monitored at 436nm and the spent beads are discarded. Packing another resin mini-column in the flow cell and repeating the concentration step it is possible to carried out the mercury determination by using Dithizone as reagent. The absorbance of the Dithizone-Hg complex is monitored at 500nm. After each measurement, the spent beads are wasted and a new portion of fresh one is trapped in the system, letting it ready for the next measurement. The bead injection system is versatile and can be used to concentrate different sample volumes, which permits the determination of a wide range of copper and mercury ions concentrations. When the sample-selected volumes are 100 and 1000mul the analytical ranges were 5.0 up to 500.0mugl(-1) and 2.5 up to 30.0mugl(-1) for Cu(II) and Hg(II) ions, respectively. Under these conditions, the detection limit was estimated as 0.63 and 0.25mugl(-1) for copper and mercury ions determination. The system consumes 2mg of Chelex 100 resin beads, 0.20mg of APDC or 1.25mg of Dithizone per determination and the traditional organic solvent extraction methodology, normally used in connection

  13. Application of factorial design and Doehlert matrix for determination of trace lead in environmental samples by on-line column preconcentration FAAS using silica gel chemically modified with niobium(V) oxide.

    PubMed

    Roux, Kalya Cravo Di Pietro; Maltez, Heloisa França; Carletto, Jeferson Schneider; Martendal, Edmar; Carasek, Eduardo

    2008-03-01

    In this study a new method for Pb determination in water using solid phase extraction coupled to a flow injection system and flame atomic absorption spectrometry was developed. The sorbent used for Pb preconcentration and extraction was silica gel chemically modified with niobium(V) oxide. Flow and chemical variables of the system were optimized through a multivariate procedure. The factors selected were buffer type, eluent concentration, and sample and eluent flow rates. It was verified that the aforementioned factors as well as their interactions were statistically significant at the 95% confidence level. The effect of foreign ions was evaluated using a fractionary factorial experimental design. The detection limit was 0.35 microg L(-1) and the precision was 1.6%. Results for recovery tests using different environmental samples were between 90 and 104%. Certified reference materials were analyzed in order to check the accuracy of the proposed method. PMID:18332544

  14. Tortuous path chemical preconcentrator

    DOEpatents

    Manginell, Ronald P.; Lewis, Patrick R.; Adkins, Douglas R.; Wheeler, David R.; Simonson, Robert J.

    2010-09-21

    A non-planar, tortuous path chemical preconcentrator has a high internal surface area having a heatable sorptive coating that can be used to selectively collect and concentrate one or more chemical species of interest from a fluid stream that can be rapidly released as a concentrated plug into an analytical or microanalytical chain for separation and detection. The non-planar chemical preconcentrator comprises a sorptive support structure having a tortuous flow path. The tortuosity provides repeated twists, turns, and bends to the flow, thereby increasing the interfacial contact between sample fluid stream and the sorptive material. The tortuous path also provides more opportunities for desorption and readsorption of volatile species. Further, the thermal efficiency of the tortuous path chemical preconcentrator is comparable or superior to the prior non-planar chemical preconcentrator. Finally, the tortuosity can be varied in different directions to optimize flow rates during the adsorption and desorption phases of operation of the preconcentrator.

  15. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection.

    PubMed

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-06-15

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra-trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed. The samples are adjusted to pH 5.0 on-line in the system for optimum operation. The target ions are adsorbed by chelation on the surface of the beads, contained in a 20mul microcolumn within the LOV, and following elution by 50mul 2M nitric acid, the eluate is, as sandwiched by air segments, introduced into the ETAAS. Based on the consumption of 1.8ml sample solution, retention efficiencies of 95, 75 and 90%, enrichment factors of 34, 27 and 32, and determination limits of 0.001, 0.07 and 0.02mugl(-1) were obtained for Cd(II), Pb(II) and Ni(II), respectively. The beads can be used repeatedly for at least 20 times without decrease of performance, yet can be replaced at will if the circumstances should so dictate. The optimized procedural parameters showed that 12 samples per hour could be prepared and successfully analyzed. The results obtained for three standard reference materials agreed very well with the certified values.

  16. Development of a miniature analytical system in a lab-on-valve for determination of trace copper by bead injection spectroscopy.

    PubMed

    Yu, Yong-Liang; Jiang, Ying; He, Rong-Huan

    2012-01-15

    A miniature analytical system based on a lab-on-valve platform is developed for trace metal analysis by bead injection spectroscopy. A multipurpose flow cell integrated into a lab-on-valve is furnished with two pieces of fiber optics to communicate with light source and charge coupled device (CCD) spectrometer, respectively, in order to monitor real-time absorbance of the samples. Micro-beads loaded with chromogenic reagent are packed into the multipurpose flow cell to form a renewable microcolumn for solid phase extraction by bead injection. When the sample solution flows through the microcolumn, the target analyte will be captured on the surface of beads and detected directly by the CCD spectrometer without elution. The beads are automatically discarded from the multipurpose flow cell after each analytical cycle. This analytical system was employed to determine trace copper by loading of a chromogenic reagent 2-carboxy-2'-hydroxy-5'-sulfoformazylbenzene (zincon) on the beads of an anion exchanger (Sephadex QAE A-25). With a sample volume of 2.5mL, a detection limit of 3μgL(-1) and a linear range of 10-100μgL(-1) were obtained for copper, along with a RSD value of 2.5% (at the 50μgL(-1) level). The accuracy and practical applicability of the proposed system were validated by analysing certified reference materials, i.e., GBW10010, GBW09101, GBW08608, and further demonstrated by spiking recovery of copper in a water sample.

  17. Methods for improved preconcentrators

    DOEpatents

    Manginell, Ronald P.; Lewis, Patrick R.; Okandan, Murat

    2010-06-01

    The present invention relates generally to chemical analysis (e.g. by gas chromatography), and in particular to a compact chemical preconcentrator formed on a substrate with a heatable sorptive membrane that can be used to accumulate and concentrate one or more chemical species of interest over time and then rapidly release the concentrated chemical species upon demand for chemical analysis.

  18. Determination of salivary cotinine through solid phase extraction using a bead-injection lab-on-valve approach hyphenated to hydrophilic interaction liquid chromatography.

    PubMed

    Ramdzan, Adlin N; Barreiros, Luísa; Almeida, M Inês G S; Kolev, Spas D; Segundo, Marcela A

    2016-01-15

    Cotinine, the first metabolite of nicotine, is often used as a biomarker in the monitoring of environmental tobacco smoke (ETS) exposure due to its long half-life. This paper reports on the development of an at-line automatic micro-solid phase extraction (μSPE) method for the determination of salivary cotinine followed by its analysis via hydrophilic interaction liquid chromatography (HILIC). The SPE methodology is based on the bead injection (BI) concept in a mesofluidic lab-on-valve (LOV) flow system to automatically perform all SPE steps. Three commercially available reversed-phase sorbents were tested, namely, Oasis HLB, Lichrolut EN and Focus, and the spherically shaped sorbents (i.e., Oasis HLB and Focus) provided better packing within the SPE column and hence higher column efficiency. An HILIC column was chosen based on its potential for achieving higher sensitivity and better retention of polar compounds such as cotinine. The method uses an isocratic program with acetonitrile:100mM ammonium acetate buffer, pH 5.8 in 95:5 v/v ratio as the mobile phase at a flow rate of 1.0 mL min(-1). Using this approach, the linear calibration range was from 10 to 1000 ng which corresponded to 5-500 μg L(-1). The corresponding μSPE-BI-LOV system was proven to be reliable in the handing and analysis of viscous biological samples such as saliva, achieving a sampling rate of 6h(-1) and a limit of detection and quantification of 1.5 and 3μgL(-1), respectively. PMID:26747690

  19. Human portable preconcentrator system

    DOEpatents

    Linker, Kevin L.; Bouchier, Francis A.; Hannum, David W.; Rhykerd, Jr., Charles L.

    2003-01-01

    A preconcentrator system and apparatus suited to human portable use wherein sample potentially containing a target chemical substance is drawn into a chamber and through a pervious screen. The screen is adapted to capture target chemicals and then, upon heating, to release those chemicals into the chamber. Chemicals captured and then released in this fashion are then carried to a portable chemical detection device such as a portable ion mobility spectrometer. In the preferred embodiment, the means for drawing sample into the chamber comprises a reversible fan which, when operated in reverse direction, creates a backpressure that facilitates evolution of captured target chemicals into the chamber when the screen is heated.

  20. Non-planar chemical preconcentrator

    DOEpatents

    Manginell, Ronald P.; Adkins, Douglas R.; Sokolowski, Sara S.; Lewis, Patrick R.

    2006-10-10

    A non-planar chemical preconcentrator comprises a high-surface area, low mass, three-dimensional, flow-through sorption support structure that can be coated or packed with a sorptive material. The sorptive material can collect and concentrate a chemical analyte from a fluid stream and rapidly release it as a very narrow temporal plug for improved separations in a microanalytical system. The non-planar chemical preconcentrator retains most of the thermal and fabrication benefits of a planar preconcentrator, but has improved ruggedness and uptake, while reducing sorptive coating concerns and extending the range of collectible analytes.

  1. Human portable preconcentrator system

    DOEpatents

    Linker, Kevin L.; Brusseau, Charles A.; Hannum, David W.; Puissant, James G.; Varley, Nathan R.

    2003-08-12

    A preconcentrator system and apparatus suited to human portable use wherein sample potentially containing a target chemical substance is drawn into a chamber and through a pervious screen. The screen is adapted to capture target chemicals and then, upon heating, to release those chemicals into the chamber. Chemicals captured and then released in this fashion are then carried to a portable chemical detection device such as a portable ion mobility spectrometer. In the preferred embodiment, the means for drawing sample into the chamber comprises a reversible fan which, when operated in reverse direction, creates a backpressure that facilitates evolution of captured target chemicals into the chamber when the screen is heated. The screen can be positioned directly in front of the detector prior to heating to improve detection capability.

  2. Integrating preconcentrator heat controller

    DOEpatents

    Bouchier, Francis A.; Arakaki, Lester H.; Varley, Eric S.

    2007-10-16

    A method and apparatus for controlling the electric resistance heating of a metallic chemical preconcentrator screen, for example, used in portable trace explosives detectors. The length of the heating time-period is automatically adjusted to compensate for any changes in the voltage driving the heating current across the screen, for example, due to gradual discharge or aging of a battery. The total deposited energy in the screen is proportional to the integral over time of the square of the voltage drop across the screen. Since the net temperature rise, .DELTA.T.sub.s, of the screen, from beginning to end of the heating pulse, is proportional to the total amount of heat energy deposited in the screen during the heating pulse, then this integral can be calculated in real-time and used to terminate the heating current when a pre-set target value has been reached; thereby providing a consistent and reliable screen temperature rise, .DELTA.T.sub.s, from pulse-to-pulse.

  3. [In situ photopolymerization of polyacrylamide-based preconcentrator on a microfluidic chip for capillary electrophoresis].

    PubMed

    Yamamoto, Sachio

    2012-01-01

    Microchip electrophoresis is widely used for microfluidics and has been studied extensively over the past decade. Translation of capillary electrophoresis methods from traditional capillary systems to a microchip platform provides rapid separation and easy quantitation of sample components. However, most microfluidic systems suffer from critical scaling problems. One promising solution to this problem is online sample preconcentration of all analytes in a sample reservoir before the separation channel. Herein, the following three techniques for online preconcentration during microchip electrophoresis are proposed: (1) in situ fabrication of an ionic polyacrylamide-based preconcentrator on a simple poly(methyl methacrylate) microfluidic chip for perm-selective preconcentration and capillary electrophoretic separation of anionic compounds, (2) simultaneous concentration enrichment and electrophoretic separation of weak acids on a microchip using an in situ photopolymerized carboxylate-type polyacrylamide gels as the perm-selective preconcentrator, and (3) microchip electrophoresis of oligosaccharides using lectin-immobilized preconcentrator gels fabricated by in situ photopolymerization. These techniques are expected to be powerful tools for clinical and pharmaceutical studies with on-line preconcentration during microchip electrophoresis.

  4. [In situ photopolymerization of polyacrylamide-based preconcentrator on a microfluidic chip for capillary electrophoresis].

    PubMed

    Yamamoto, Sachio

    2012-01-01

    Microchip electrophoresis is widely used for microfluidics and has been studied extensively over the past decade. Translation of capillary electrophoresis methods from traditional capillary systems to a microchip platform provides rapid separation and easy quantitation of sample components. However, most microfluidic systems suffer from critical scaling problems. One promising solution to this problem is online sample preconcentration of all analytes in a sample reservoir before the separation channel. Herein, the following three techniques for online preconcentration during microchip electrophoresis are proposed: (1) in situ fabrication of an ionic polyacrylamide-based preconcentrator on a simple poly(methyl methacrylate) microfluidic chip for perm-selective preconcentration and capillary electrophoretic separation of anionic compounds, (2) simultaneous concentration enrichment and electrophoretic separation of weak acids on a microchip using an in situ photopolymerized carboxylate-type polyacrylamide gels as the perm-selective preconcentrator, and (3) microchip electrophoresis of oligosaccharides using lectin-immobilized preconcentrator gels fabricated by in situ photopolymerization. These techniques are expected to be powerful tools for clinical and pharmaceutical studies with on-line preconcentration during microchip electrophoresis. PMID:23023420

  5. Mass-sensitive chemical preconcentrator

    DOEpatents

    Manginell, Ronald P.; Adkins, Douglas R.; Lewis, Patrick R.

    2007-01-30

    A microfabricated mass-sensitive chemical preconcentrator actively measures the mass of a sample on an acoustic microbalance during the collection process. The microbalance comprises a chemically sensitive interface for collecting the sample thereon and an acoustic-based physical transducer that provides an electrical output that is proportional to the mass of the collected sample. The acoustic microbalance preferably comprises a pivot plate resonator. A resistive heating element can be disposed on the chemically sensitive interface to rapidly heat and release the collected sample for further analysis. Therefore, the mass-sensitive chemical preconcentrator can optimize the sample collection time prior to release to enable the rapid and accurate analysis of analytes by a microanalytical system.

  6. Innovative combination of QuEChERS extraction with on-line solid-phase extract purification and pre-concentration, followed by liquid chromatography-tandem mass spectrometry for the determination of non-steroidal anti-inflammatory drugs and their metabolites in sewage sludge.

    PubMed

    Rossini, D; Ciofi, L; Ancillotti, C; Checchini, L; Bruzzoniti, M C; Rivoira, L; Fibbi, D; Orlandini, S; Del Bubba, M

    2016-09-01

    For the first time QuEChERS extraction of sewage sludge was combined with the automatic solid-phase pre-concentration and purification of the extract (following indicated as SPE) and LC-MS/MS analysis, for the determination of the non-steroidal anti-inflammatory drugs acetylsalicylic acid (ASA), diclofenac (DIC), fenbufen (FEN), flurbiprofen (FLU), ketoprofen (KET), ibuprofen (IBU) and naproxen (NAP), and their metabolites salicylic acid (SAL), 4'-hydroxydiclofenac (4'-HYDIC), 1-hydroxyibuprofen (1-HYIBU), 2-hydroxyibuprofen (2-HYIBU), 3-hydroxyibuprofen (3-HYIBU) and o-desmethylnaproxen (O-DMNAP). Various commercial pellicular stationary phases (i.e. silica gel functionalized with octadecyl, biphenyl, phenylhexyl and pentafluorophenyl groups) were preliminarily investigated for the resolution of target analytes and different sorbent phases (i.e. octyl or octadecyl functionalized silica gel and a polymeric phase functionalized with N-benzylpyrrolidone groups) were tested for the SPE phase. The optimized method involves the QuEChERS extraction of 1 g of freeze-dried sludge with 15 mL of water/acetonitrile 1/2 (v/v), the SPE of the extract with the N-benzylpyrrolidone polymeric phase and the water/acetonitrile gradient elution on the pentafluorophenyl stationary phase at room temperature. Matrix effect was always suppressive and in most cases low, being it ≤20% for ASA, DIC, FLU, KET, IBU, 1-HYIBU, 2-HYIBU, 3-HYIBU, NAP and O-DMNAP, and included in the range of 35-47% for the other analytes. Recoveries were evaluated at three spiking levels, evidencing almost quantitative values for HYIBUs and O-DMNAP; for ASA, SAL and KET the recoveries were included in between 50 and 76%, whereas for the other compounds they ranged from 36% to 55%. The proposed method showed better analytical performances than those so far published, being suitable for target compound determination in real samples from tens of pg g(-1) to ng g(-1) of freeze-dried sludge, with a total analysis

  7. Chemical preconcentrator with integral thermal flow sensor

    DOEpatents

    Manginell, Ronald P.; Frye-Mason, Gregory C.

    2003-01-01

    A chemical preconcentrator with integral thermal flow sensor can be used to accurately measure fluid flow rate in a microanalytical system. The thermal flow sensor can be operated in either constant temperature or constant power mode and variants thereof. The chemical preconcentrator with integral thermal flow sensor can be fabricated with the same MEMS technology as the rest of the microanlaytical system. Because of its low heat capacity, low-loss, and small size, the chemical preconcentrator with integral thermal flow sensor is fast and efficient enough to be used in battery-powered, portable microanalytical systems.

  8. High throughput liquid absorption preconcentrator sampling instrument

    DOEpatents

    Zaromb, Solomon; Bozen, Ralph M.

    1992-01-01

    A system for detecting trace concentrations of an analyte in air includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container comprising a wettable material. The wettable material is continuously wetted with an analyte-sorbing liquid which flows from one part of the container to a lower end. Sampled air flows through the container in contact with the wetted material with a swirling motion which results in efficient transfer of analyte vapors or aerosol particles to the sorbing liquid and preconcentration of traces of analyte in the liquid. The preconcentrated traces of analyte may be either detected within the container or removed therefrom for injection into a separate detection means or for subsequent analysis.

  9. Highly sensitive immunosensor using a nanofluidic preconcentrator.

    PubMed

    Liao, Ke-Pan; Sung, Kung-Bin

    2008-01-01

    This paper presents a micro-/nanofluidic biochip for enhanced sensitivity of immunoassay. By using a protein preconcentrator based on nanofluidic filters, we greatly improve the binding kinetics of immunoassay. A shallow nanofluidic channel connecting two microchannels for ion-selective filter is etched on the glass surface and sealed by PDMS/Glass irreversible bonding treated with O2 plasma. Our device achieved a 10(5) fold increase in protein concentration with 12 minutes of preconcentration. For applying the preconcentrator to immunoassay, we fabricated a novel device with a thin layer of Au sputtered near the nanochannel to provide a substrate for antibody immobilization and a sensing area at the site of highly concentrated proteins. After increasing the concentration of antibody and target antigen by multiple sample preconcentration steps, the binding kinetics of immunoassay can be significantly improved.

  10. High throughput liquid absorption preconcentrator sampling instrument

    DOEpatents

    Zaromb, S.; Bozen, R.M.

    1992-12-22

    A system for detecting trace concentrations of an analyte in air includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container comprising a wettable material. The wettable material is continuously wetted with an analyte-sorbing liquid which flows from one part of the container to a lower end. Sampled air flows through the container in contact with the wetted material with a swirling motion which results in efficient transfer of analyte vapors or aerosol particles to the sorbing liquid and preconcentration of traces of analyte in the liquid. The preconcentrated traces of analyte may be either detected within the container or removed therefrom for injection into a separate detection means or for subsequent analysis. 12 figs.

  11. On-Line Cataloging.

    ERIC Educational Resources Information Center

    OCLC Online Computer Library Center, Inc., Dublin, OH.

    The principal objective of the Ohio College Library Center is to lower the rate of rise of per-unit library costs while increasing the availability of library resources for use by patrons of participating libraries. A major procedural goal of the on-line cataloging system is to furnish cataloging personnel in individual libraries with…

  12. Large-volume sampling and preconcentration for trace explosives detection.

    SciTech Connect

    Linker, Kevin Lane

    2004-05-01

    A trace explosives detection system typically contains three subsystems: sample collection, preconcentration, and detection. Sample collection of trace explosives (vapor and particulate) through large volumes of airflow helps reduce sampling time while increasing the amount of dilute sample collected. Preconcentration of the collected sample before introduction into the detector improves the sensitivity of the detector because of the increase in sample concentration. By combining large-volume sample collection and preconcentration, an improvement in the detection of explosives is possible. Large-volume sampling and preconcentration is presented using a systems level approach. In addition, the engineering of large-volume sampling and preconcentration for the trace detection of explosives is explained.

  13. Sample preconcentration with chemical derivatization in capillary electrophoresis. Capillary as preconcentrator, microreactor and chiral selector for high-throughput metabolite screening.

    PubMed

    Ptolemy, Adam S; Britz-McKibbin, Philip

    2006-02-17

    New strategies for integrating sample pretreatment with chemical analyses under a single format is required for rapid, sensitive and enantioselective analyses of low abundance metabolites in complex biological samples. Capillary electrophoresis (CE) offers a unique environment for controlling analyte/reagent band dispersion and electromigration properties using discontinuous electrolyte systems. Recent work in our laboratory towards developing a high-throughput CE platform for low abundance metabolites via on-line sample preconcentration with chemical derivatization (SPCD) is primarily examined in this review, as there have been surprisingly only a few strategies reported in the literature to date. In-capillary sample preconcentration serves to enhance concentration sensitivity via electrokinetic focusing of long sample injection volumes for lower detection limits, whereas chemical derivatization by zone passing is used to expand detectability and selectivity, notably for enantiomeric resolution of metabolites lacking intrinsic chromophores using nanolitre volumes of reagent. Together, on-line SPCD-CE can provide over a 100-fold improvement in concentration sensitivity, shorter total analysis times, reduced sample handling and improved reliability for a variety of amino acid and amino sugar metabolites, which is also amenable to automated high-throughput screening. This review will highlight basic method development and optimization parameters relevant to SPCD-CE, including applications to bacterial metabolite flux and biomarker analyses. Insight into the mechanism of analyte focusing and labeling by SPCD-CE is also discussed, as well as future directions for continued research.

  14. Sample preconcentration with chemical derivatization in capillary electrophoresis. Capillary as preconcentrator, microreactor and chiral selector for high-throughput metabolite screening.

    PubMed

    Ptolemy, Adam S; Britz-McKibbin, Philip

    2006-02-17

    New strategies for integrating sample pretreatment with chemical analyses under a single format is required for rapid, sensitive and enantioselective analyses of low abundance metabolites in complex biological samples. Capillary electrophoresis (CE) offers a unique environment for controlling analyte/reagent band dispersion and electromigration properties using discontinuous electrolyte systems. Recent work in our laboratory towards developing a high-throughput CE platform for low abundance metabolites via on-line sample preconcentration with chemical derivatization (SPCD) is primarily examined in this review, as there have been surprisingly only a few strategies reported in the literature to date. In-capillary sample preconcentration serves to enhance concentration sensitivity via electrokinetic focusing of long sample injection volumes for lower detection limits, whereas chemical derivatization by zone passing is used to expand detectability and selectivity, notably for enantiomeric resolution of metabolites lacking intrinsic chromophores using nanolitre volumes of reagent. Together, on-line SPCD-CE can provide over a 100-fold improvement in concentration sensitivity, shorter total analysis times, reduced sample handling and improved reliability for a variety of amino acid and amino sugar metabolites, which is also amenable to automated high-throughput screening. This review will highlight basic method development and optimization parameters relevant to SPCD-CE, including applications to bacterial metabolite flux and biomarker analyses. Insight into the mechanism of analyte focusing and labeling by SPCD-CE is also discussed, as well as future directions for continued research. PMID:16336972

  15. Separation preconcentration method for platinum and rhodium from environmental samples using a chelating resin.

    PubMed

    Bosch Ojeda, C; Sánchez Rojas, F; Cano Pavón, J M

    2006-01-01

    A method of determining trace levels of platinum and rhodium in different samples was investigated. The method involves separation and preconcentration of the platinum and rhodium from the matrix by flow injection (FI) on-line coupled with electrothermal atomic absorption spectrometry (ETAAS) with Zeeman effect background correction. Platinum and rhodium were adsorbed on a microcolumn packed with 1,5-bis(di-2-pyridyl)methylene thiocarbohydrazide immobilized on silica gel (DPTH-gel). The sorbed metals were directly eluted with nitric acid into the graphite furnace and determined by AAS.

  16. Preconcentration of phenols by fibrous sorbents

    SciTech Connect

    Andreeva, I.Yu.; Kuvaldina, L.L.

    1995-01-01

    Phenols are among the most toxic contaminants of natural and waste waters. There are standard procedures for determining them in low concentrations. However, the samples cannot be preserved at phenol concentrations of 50 {mu}g/L or lower, and the determination of phenols must be performed no later than 2 h after sampling. This is not always possible. Because of this, the preconcentration of phenols at the site of sampling, followed by analysis of the concentrate in a stationary chemical laboratory after a time, is of interest. The technique of phenol preconcentration with active carbon, recommended in the standard procedure, is unsuitable for these purposes because the adsorption and desorption of phenols are too prolonged. At the same time, a fibrous carbon sorbent provides for a high rate of adsorption and desorption of some organic substances (humic acids, fulvic acids, and surfactants) it can be easily regenerated and repeatedly used. In this work, the authors investigated the possibility of using two fibers-namely, a carbon fiber and a polyethylene-polyamine-modified polyacrylonitrile-based fiber (PAN-PEA) containing amino groups with different numbers of substituents-for the preconcentration of phenols.

  17. Liquid-absorption preconcentrator sampling instrument

    DOEpatents

    Zaromb, S.

    1990-12-11

    A system is described for detecting trace concentrations of an analyte in air and includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container in which is disposed a wettable material extending substantially the entire length of the container. One end of the wettable material is continuously wetted with an analyte-sorbing liquid, which flows to the other end of the container. Sample air is flowed through the container in contact with the wetted material for trapping and preconcentrating the traces of analyte in the sorbing liquid, which is then collected at the other end of the container and discharged to the detector. The wetted material may be a wick comprising a bundle of fibers, one end of which is immersed in a reservoir of the analyte-sorbing liquid, or may be a liner disposed on the inner surface of the container, with the sorbing liquid being centrifugally dispersed onto the liner at one end thereof. The container is preferably vertically oriented so that gravity effects the liquid flow. 4 figs.

  18. Liquid-absorption preconcentrator sampling instrument

    DOEpatents

    Zaromb, Solomon

    1990-01-01

    A system for detecting trace concentrations of an analyte in air and includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container in which is disposed a wettable material extending substantially the entire length of the container. One end of the wettable material is continuously wetted with an analyte-sorbing liquid, which flows to the other end of the container. Sample air is flowed through the container in contact with the wetted material for trapping and preconcentrating the traces of analyte in the sorbing liquid, which is then collected at the other end of the container and discharged to the detector. The wetted material may be a wick comprising a bundle of fibers, one end of which is immersed in a reservoir of the analyte-sorbing liquid, or may be a liner disposed on the inner surface of the container, with the sorbing liquid being centrifugally dispersed onto the liner at one end thereof. The container is preferably vertically oriented so that gravity effects the liquid flow.

  19. A MEMS Based Hybrid Preconcentrator/Chemiresistor Chemical Sensor

    SciTech Connect

    HUGHES,ROBERT C.; PATEL,SANJAY V.; MANGINELL,RONALD P.

    2000-06-12

    A hybrid of a microfabricated planar preconcentrator and a four element chemiresistor array chip has been fabricated and the performance as a chemical sensor system has been demonstrated. The close proximity of the chemiresistor sensor to the preconcentrator absorbent layer allows for fast transfer of the preconcentrated molecules during the heating and resorption step. The hybrid can be used in a conventional flow sampling system for detection of low concentrations of analyte molecules or in a pumpless/valveless mode with a grooved lid to confine the desorption plume from the preconcentrator during heating.

  20. Continuous approach for ultrasound-assisted acid extraction-minicolumn preconcentration of chromium and cobalt from seafood samples prior to flame atomic absorption spectrometry.

    PubMed

    Yebra-Biurrun, Maria C; Cancela-Pérez, Sheila

    2007-08-01

    A rapid and sensitive method has been proposed for the determination of chromium and cobalt in seafood samples by flame atomic absorption spectrometry combined with a dynamic ultrasound-assisted acid extraction and an on-line minicolumn preconcentration. The use of diluted nitric acid as extractant in a continuous mode at a flow rate of 3.5 mL min(-1) and room temperature was sufficient for quantitative extraction of these trace metals from seafoods. A minicolumn containing a chelating resin was an excellent device for the quantitative preconcentration of chromium and cobalt prior to their detection. A flow-injection manifold was used as interface for coupling all analytical steps, which allowed the automation of the whole analytical process. A Plackett-Burman experimental design was used as a multivariate strategy for the optimization of both sample preparation and preconcentration steps. The method was successfully applied to the determination of chromium and cobalt in seafood samples.

  1. Online microchannel preconcentrator for carbofuran detection.

    PubMed

    Siritham, Charinrat; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

    2013-01-01

    A simple and rapid online microchannel preconcentrator coupled with an amperometric detection for the analysis of carbofuran using polyethylene glycol coated onto magnetic particle (PEG-magnetic particles) sorbents was developed. This simple-to-prepare microchannel preconcentrator used an external magnet to retain the PEG-magnetic particle sorbents inside the microchannel. Under optimum conditions, the system provided two linear ranges, from 0.01 to 10.0 mg L(-1) and from 10.0 to 130.0 mg L(-1) with a limit of detection of 8.7 ± 0.1 μg L(-1). The microchannel preconcentrator provided very good stability; it can be used for up to 326 consecutive injections of 5.0 mg L(-1) carbofuran with a relative standard deviation of less than 3%. The developed system provided a good microchannel-to-microchannel and a good electrode-to-electrode reproducibility (n = 6, %RSD < 1). It also provided an excellent selectivity when it was tested with two other carbamate pesticides, carbaryl and methomyl, with a 43 and 256 times higher detection sensitivity for carbofuran, respectively. The developed system was successfully applied to detect carbofuran in surface water samples obtained near vegetable plantation areas. The concentrations of carbofuran in these samples were found to be in the range of non-detectable to 0.047 ± 0.001 mg L(-1). The developed system is easy to operate and easy to couple with other analytical instruments and it could be easily adapted for the analysis of other polar organic contaminants.

  2. Odor Sensing System Using Preconcentrator with Variable Temperature

    SciTech Connect

    Isaka, Y; Nakamoto, Takamichi; Moriizumi, T; Grate, Jay W. )

    1999-01-01

    An odor sensing system using QCM gas sensor array and pattern recognition technique is useful to identify various kinds of odors. A preconcentrator with variable temperature is promising to obtain further pattern separation after the appropriate temperature changes, whereas it has been so far used to enhance sensor sensitivity. After the preconcentrator collects the vapors, it is heated so that they can be thermally desorbed. The combination of the preconcentrator with the sensor array enhances the capability of discrimination among vapors since their desorption temperatures depend upon vapor kinds.

  3. Sample preconcentration inside sessile droplets using electrowetting

    PubMed Central

    Mampallil, Dileep; Tiwari, Dhirendra; van den Ende, Dirk; Mugele, Frieder

    2013-01-01

    Electrowetting with alternate voltage (AC) creates azimuthal flow vortices inside sessile droplets. These flow vortices can be controlled by introducing pinning sites at the contact line. When the frequency of the applied AC voltage is gradually ramped from a few hundreds of hertz to a few tens of kilohertz the azimuthal flow vortices contract and move towards the contact line near the pinning site. Dispersed particles in the liquid are collected in the center of these vortices leading to an increase in the local particle concentration by up to more than one order of magnitude. We provide a qualitative explanation for symmetry of the flow patterns within the drops and discuss possible scenarios explaining the particle collection and preconcentration. PMID:24404036

  4. On-Line Communications Devices.

    ERIC Educational Resources Information Center

    Sternick, Barbara R.

    These summaries have been compiled to assist users in selecting terminals for use with the National Library of Medicine (NLM) on-line systems. The summaries describe the salient characteristics and approximate prices of a large number of hard copy and display devices. Many of the terminals listed may be modified by the addition of various options…

  5. On-line monitoring of diatom lysis by thermal lens spectrometry

    NASA Astrophysics Data System (ADS)

    Logar, J. K.; Malej, A.; Franko, M.

    2005-06-01

    The applicability of a double dual beam thermal lens spectrometer in on-line monitoring of phytoplankton cell lysis was tested in laboratory experiments with cultured diatom Skeletonema costatum. The lysis was induced by the addition of the cytotoxin poly-APS. Increased poly-APS concentration resulted in increased cell lysis and release of cellular pigments into the solution. The associated change in absorbance was monitored as increased difference of TLS signals from lysed and control cultures. The lowest number of decayed cells that can be detected by the double dual beam TLS without any pretreatment or preconcentration of the examined culture is 6.106 to 107 cells/L.

  6. High-throughput liquid-absorption preconcentrator sampling methods

    DOEpatents

    Zaromb, Solomon

    1994-01-01

    A system for detecting trace concentrations of an analyte in air includes a preconcentrator for the analyte and an analyte detector. The preconcentrator includes an elongated tubular container comprising a wettable material. The wettable material is continuously wetted with an analyte-sorbing liquid which flows from one part of the container to a lower end. Sampled air flows through the container in contact with the wetted material with a swirling motion which results in efficient transfer of analyte vapors or aerosol particles to the sorbing liquid and preconcentration of traces of analyte in the liquid. The preconcentrated traces of analyte may be either detected within the container or removed therefrom for injection into a separate detection means or for subsequent analysis.

  7. Online Preconcentration and Determination of Trace Amounts of Zinc in Nature Waters

    PubMed Central

    Wei, Liang; Zhang, Xinshen; Dai, Yichun; Huang, Jin; Xie, Yong-hong; Xiao, Kai

    2008-01-01

    A simple, sensitive, reliable and flexible flow injection spectrophotometric method is proposed for on-line preconcentration and determination of trace amounts of zinc in water. At the presence of Tween-80 in pH 9.3 buffer solutions, the shade of color of Zn (II)-PAN complex is in a linear relation to the zinc amount at the point of the maximum absorption peak of 560 nm. The optimal experimental conditions, including reaction conditions and preconcentration conditions, had been obtained. The linear range of the proposed method was between 2.0 and 360 μg L−1 and the detection limit was 0.42 μg L−1. The relative standard deviation was 3.55% and 2.14% for 5.0 μg L−1 and 50 μg L−1 of zinc standard solution (n = 8). The method had been successfully applied to zinc determination in water samples and the analytical results were satisfactory. PMID:18389074

  8. Magnetic materials as sorbents for metal/metalloid preconcentration and/or separation. A review.

    PubMed

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-07-30

    The use of magnetic materials in solid phase extraction has received considerable attention in recent years taking into account many advantages arising from the inherent characteristics of magnetic particles. Magnetic solid phase extraction (MSPE) methodology overcomes problems such as column packing and phase separation, which can be easily performed by applying an external magnetic field. The use of magnetic particles in automatic systems is growing over the last few years making the on-line operation of MSPE a promising technique in the frame of green chemistry. This article aims to provide all recent progress in the research of novel magnetic materials as sorbents for metal preconcentration and determination coupled with different detection systems as well as their implementation in sequential injection and microfluidic systems. In addition, a description of preparation, characterization as well as applications of various types of magnetic materials, either with organic or inorganic coating of the magnetic core, is presented. Concluding remarks and future trends are also commented.

  9. Evaluation of chelation preconcentration for the determination of actinide elements by flow injection ICP-MS

    SciTech Connect

    Evans, E.H.; Truscott, J.B.; Bromley, L.; Jones, P.; Turner, J.; Fairman, B.E.

    1998-12-31

    A chelation column preconcentration method has been developed for the determination of uranium and thorium in waters by ICP-MS. Detection limits of 24 pg and 60 pg respectively were obtained, but these were blank limited. Uranium and Thorium were determined in certified reference materials. Results for uranium were 121 {+-} 21 and 15 {+-} 3 ng/g in NIST 1566a and NIST 1575 compared with certified values of 132 {+-} 12 and 20 {+-} 4 ng/g respectively. Results for thorium were 29 {+-} 8 and 28 {+-} 5 ng/g in NIST 1566a and NIST 1575 compared with indicative and certified values of 40 and 37 {+-} 3 ng/g respectively. The on-line separation of actinide radionuclides was achieved by selective elution of U, Th, Pu, Np, and Am.

  10. Dynamic pH junction preconcentration in capillary electrophoresis- electrospray ionization-mass spectrometry for proteomics analysis.

    PubMed

    Zhu, Guijie; Sun, Liangliang; Dovichi, Norman J

    2016-09-21

    Capillary zone electrophoresis (CZE)-electrospray ionization (ESI)-mass spectrometry (MS) is an interesting complimentary technique to reversed phase liquid chromatography (RPLC)-ESI-MS for proteomics research. However, the low sample loading capacity of CZE (typically a few nL) can limit its application for large-scale proteomics. A number of on-line sample preconcentration methods have been developed to increase sample loading volumes. This review considers the dynamic pH junction as a simple on-line sample preconcentration method; this method is well suited for amphiprotic analytes. In the pH junction, these analytes are suspended in a basic buffer, injected by pressure into the capillary, and separated in an acidic background electrolyte, with no changes in either CZE-MS operations or instrumentation. We have demonstrated that the dynamic pH junction method can improve the sample loading volume to sub-μL volumes without significant loss of separation capacity for bottom-up proteomic analysis. The dynamic pH junction based CZE-ESI-MS system has been applied for a number of complex biological samples, including the E. coli proteome, impurities in recombinant antibody therapeutics, and the characterization of the phosphoproteome from a human cell line. PMID:27460877

  11. On-line surfactant monitoring

    SciTech Connect

    Mullen, K.I.; Neal, E.E.; Soran, P.D.; Smith, B.

    1995-04-01

    This group has developed a process to extract metal ions from dilute aqueous solutions. The process uses water soluble polymers to complex metal ions. The metal/polymer complex is concentrated by ultrafiltration and the metals are recovered by a pH adjustment that frees the metal ions. The metal ions pass through the ultrafiltration membrane and are recovered in a concentrated form suitable for reuse. Surfactants are present in one of the target waste streams. Surfactants foul the costly ultrafiltration membranes. It was necessary to remove the surfactants before processing the waste stream. This paper discusses an on-line device the authors fabricated to monitor the process stream to assure that all the surfactant had been removed. The device is inexpensive and sensitive to very low levels of surfactants.

  12. Two-stage preconcentrator for vapor/particle detection

    DOEpatents

    Linker, Kevin L.; Brusseau, Charles A.

    2002-01-01

    A device for concentrating particles from a high volume gas stream and delivering the particles for detection in a low volume gas stream includes first and second preconcentrators. The first preconcentrator has a first structure for retaining particles in a first gas flow path through which a first gas flows at a relatively high volume, valves for selectively stopping the first gas flow; and a second gas flow path through which gas flows at an intermediate flow volume for moving particles from the first structure. The second preconcentrator includes a second structure for retaining particles in the second gas flow path; a valve for selectively stopping the second gas flow; and a third gas flow path through which gas flows at a low volume for moving particles from the second structure to a detector. Each of the particle retaining structures is preferably a metal screen that may be resistively heated by application of an electric potential to release the particles.

  13. The NSINIC on-line system

    NASA Technical Reports Server (NTRS)

    Lev, Brian

    1991-01-01

    The NSI NIC on-line system is described in the form of view graphs. The following subject areas are covered: NSI history; the ADFTO's other on-line services; the current system; and the next generation of NSI NIC.

  14. Solvent vapors controlled by pre-concentration, incineration

    SciTech Connect

    Sundberg, R.E.

    1996-01-01

    Concentration of solvent vapors in ventilation air exhausted from the workplace often is too dilute for efficient destruction or recovery. Several techniques are being developed to pre-concentrate the vapors before treating them in a catalytic incinerator. Molnbacka Industri AB (Forshaga, Sweden) has developed a system to control volatile organic compound emissions by using activated carbon adsorbers to pre-concentrate the solvent vapors. The technology uses carbon adsorption and desorption to concentrate dilute solvent vapors to a much smaller air stream for efficient destruction in a catalytic incinerator.

  15. Less common applications of monoliths: Preconcentration andsolid-phase extraction

    SciTech Connect

    Svec, Frantisek

    2006-03-27

    Monolithic materials are finding their place in a variety of fields. While liquid chromatography is the most emphasized use of this new category of porous media, some other just as important applications are eclipsed by the success of monolithic columns. This review article describes all current facets of use of monoliths in preconcentration and solid-phase extraction. In addition to the typical off line use that does not seem to be the main stream application for the monolithic materials, in-line connection of the preconcentration with HPLC, electrochromatography, electrophoresis, enzymatic digestion, as well as its applications in microfluidics are presented.

  16. SELF-ASSEMBLY CARBON NANOTUBES IN A MICROTRAP FOR ON-LINE PRECONCENTRATION OF VOLATILE ORGANICS. (R830901)

    EPA Science Inventory

    The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

  17. Gold volatile species atomization and preconcentration in quartz devices for atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Arslan, Yasin; Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan; Dědina, Jiří

    2015-01-01

    The on-line atomization of gold volatile species was studied and the results were compared with thermodynamic calculations in several quartz atomizers, namely: diffusion flame, flame-in-gas-shield, flame-in-plain-tube, externally heated T-tube and externally heated flame-in-T-tube. Atomization mechanism in the explored devices is proposed, where volatile species are converted to thermodynamically stable AuH at elevated temperature over 500 °C and then atomized by an interaction with a cloud of hydrogen radicals. Because of its inherent simplicity and robustness, diffusion flame was employed as a reference atomizer. It yielded atomization efficiency of 70 to 100% and a very good long time reproducibility of peak area sensitivity: 1.6 to 1.8 s μg- 1. Six and eleven times higher sensitivity, respectively, was provided by atomizers with longer light paths in the observation volume, i.e. externally heated T-tube and externally heated flame-in-T-tube. The latter one, offering limit of detection below 0.01 μg ml- 1, appeared as the most prospective for on-line atomization. Insight into the mechanism of atomization of gold volatile species, into the fate of free atoms and into subsequent analyte transfer allowed to assess possibilities of in-atomizer preconcentration of gold volatile species: it is unfeasible with quartz atomizers but a sapphire tube atomizer could be useful in this respect.

  18. PIXE analysis of preconcentrated body fluids, especially urine

    NASA Astrophysics Data System (ADS)

    Pakarinen, Pirjo; Ekholm, Ann-Kristin; Pallon, Jan

    1990-04-01

    A cation exchange resin, Chelex 100, has been used to separate and preconcentrate trace metal ions in urine. A good recovery of several metal ions in doped urine is achieved. The validity of the procedure has been checked by analyzing a certified control urine for metals, Lanonorm. The method is also applicable for amniotic fluid samples.

  19. Sample extraction and injection with a microscale preconcentrator.

    SciTech Connect

    Robinson, Alex Lockwood; Chan, Helena Kai Lun

    2007-09-01

    This report details the development of a microfabricated preconcentrator that functions as a fully integrated chemical extractor-injector for a microscale gas chromatograph (GC). The device enables parts-per-billion detection and quantitative analysis of volatile organic compounds (VOCs) in indoor air with size and power advantages over macro-scale systems. The 44 mm{sup 3} preconcentrator extracts VOCs using highly adsorptive, granular forms of graphitized carbon black and carbon molecular sieves. The micron-sized silicon cavities have integrated heating and temperature sensing allowing low power, yet rapid heating to thermally desorb the collected VOCs (GC injection). The keys to device construction are a new adsorbent-solvent filling technique and solvent-tolerant wafer-level silicon-gold eutectic bonding technology. The product is the first granular adsorbent preconcentrator integrated at the wafer level. Other advantages include exhaustive VOC extraction and injection peak widths an order of magnitude narrower than predecessor prototypes. A mass transfer model, the first for any microscale preconcentrator, is developed to describe both adsorption and desorption behaviors. The physically intuitive model uses implicit and explicit finite differences to numerically solve the required partial differential equations. The model is applied to the adsorption and desorption of decane at various concentrations to extract Langmuir adsorption isotherm parameters from effluent curve measurements where properties are unknown a priori.

  20. TEST AND EVALUATION OF A POLYMER MEMBRANE PRECONCENTRATOR

    EPA Science Inventory

    The report gives results of an evaluation of the applicability of membrane systems as a preconcentrator and defines operating parameters of a membrane system. Advantages of such a system is a potential reduction in cost for subsequent control systems. The evaluation is part of a ...

  1. Method for preconcentrating a sample for subsequent analysis

    DOEpatents

    Zaromb, Solomon

    1990-01-01

    A system for analysis of trace concentration of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

  2. Application of flow injection on-line electrothermal atomic absorption spectrometry to the determination of rhodium.

    PubMed

    Sanchez Rojas, Fuensanta; Bosch Ojeda, Catalina; Cano Pavón, José Manuel

    2005-06-01

    A fully automated procedure for the determination of rhodium has been developed using flow injection (FI) on-line microcolumn preconcentration coupled with electrothermal atomic absorption spectrometry (ETAAS). The proposed FI manifold and its operation make possible the introduction of the total eluate volume into the graphite atomizer, avoiding the necessity for optimisation of subsampling the eluate. Rhodium is adsorbed on a microcolumn packed with 1,5-bis(di-2-pyridyl)methylene thiocarbohydrazide immobilized on silica gel (DPTH-gel). Under the optimum conditions, using a 60 s preconcentration time, a sample flow rate of 3.5 mL min(-1) and an injection volume of eluent of 50 microL, a linear calibration graph was obtained from 1 to at least 40 ng mL(-1) and the detection limit was 1 ng mL(-1). The proposed method has been successfully applied to the analysis of samples. Its performance was investigated against certified reference catalyst sample SRM-2557 and by recovery measurements on spiked samples (soil, foods and beverages).

  3. Determination of uranium in seawater by flow-injection preconcentration on dodecylamidoxime-impregnated resin and spectrophotometric detection.

    PubMed

    Oguma, Koichi; Suzuki, Toshihiro; Saito, Kyoichi

    2011-06-15

    A flow injection method has been developed for the determination of uranium in seawater combining the on-line preconcentration with spectrophotometric detection. An aliquot (10 mL) of the seawater sample adjusted to pH 5.5 was injected into the analytical system and uranium was adsorbed on the column packed with styrene-divinylbenzene copolymer resin (Bio-Beads SM-2) modified with dodecylamidoxime which showed high selectivity to uranium. Uranium was then eluted with 0.01 M hydrochloric acid and detected spectrophotometrically after the reaction with Chlorophosphonazo III. Interference from calcium and strontium was masked with cyclohexanediaminetetraacetic acid added to the chromogenic reagent solution. The sample throughput, the detection limit (3σ), and the preconcentration factor were 23 per hour, 0.13 μg/L, and 20, respectively, when the sample injection volume was kept at 10 mL. The precision at the 2 μg/L level was less than 4% (RSD). The proposed method was applied to the determination of uranium in the seawater samples collected off the Boso peninsula, Japan and the uranium concentration was found to be ca. 3 μg/L, which is close to the literature data. The yield of the recovery test ranged from 95% to 99%. PMID:21641428

  4. Determination of uranium in seawater by flow-injection preconcentration on dodecylamidoxime-impregnated resin and spectrophotometric detection.

    PubMed

    Oguma, Koichi; Suzuki, Toshihiro; Saito, Kyoichi

    2011-06-15

    A flow injection method has been developed for the determination of uranium in seawater combining the on-line preconcentration with spectrophotometric detection. An aliquot (10 mL) of the seawater sample adjusted to pH 5.5 was injected into the analytical system and uranium was adsorbed on the column packed with styrene-divinylbenzene copolymer resin (Bio-Beads SM-2) modified with dodecylamidoxime which showed high selectivity to uranium. Uranium was then eluted with 0.01 M hydrochloric acid and detected spectrophotometrically after the reaction with Chlorophosphonazo III. Interference from calcium and strontium was masked with cyclohexanediaminetetraacetic acid added to the chromogenic reagent solution. The sample throughput, the detection limit (3σ), and the preconcentration factor were 23 per hour, 0.13 μg/L, and 20, respectively, when the sample injection volume was kept at 10 mL. The precision at the 2 μg/L level was less than 4% (RSD). The proposed method was applied to the determination of uranium in the seawater samples collected off the Boso peninsula, Japan and the uranium concentration was found to be ca. 3 μg/L, which is close to the literature data. The yield of the recovery test ranged from 95% to 99%.

  5. Methylmercury in water samples at the pg/L level by online preconcentration liquid chromatography cold vapor-atomic fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Brombach, Christoph-Cornelius; Chen, Bin; Corns, Warren T.; Feldmann, Jörg; Krupp, Eva M.

    2015-03-01

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography-cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation.

  6. On-Line Assessment: What, Why, How.

    ERIC Educational Resources Information Center

    Natal, Dottie

    Recent increases in the speed and accessibility of computers and networks have made it possible to administer tests on-line. On-line assessment can be conducted in a controlled setting, such as a testing center, or distributed over local area networks or the Internet to libraries and student homes, allowing students the flexibility to complete…

  7. Testing Claims for On-Line Conferences.

    ERIC Educational Resources Information Center

    Selfe, Cynthia L.; Meyer, Paul R.

    1991-01-01

    Describes an exploratory study of gender and power relationships on Megabyte University, one particular on-line conference. Finds that, although results of the study are not definite, they do suggest that gender and power are present to some extent even in on-line conferences. (MG)

  8. Flow injection analysis of water. Part 1: Automatic preconcentration determination of sulphate, ammonia and iron(II)/iron(III).

    PubMed

    Cosano, J S; de Castro, M D; Valcárcel, M

    1993-01-01

    This paper describes a simple flow-injection (FI) manifold for the determination of a variety of species in industrial water. The chemical systems involved in the determination of ammonia (formation of Indophenol Blue), sulfate (precipitation with Ba(II)), and iron (complexation with 1,10-phenanthroline with the help of a prior redox reaction for speciation) were selected so that a common manifold could be used for the sequential determination of batches of each analyte. A microcolumn of a suitable ion exchange material was used for on-line preconcentration of each analyte prior to injection; linear ranges for the determination of the analytes at the ng/ml levels were obtained with good reproducibility. The manifold and methods are ready for full automation.

  9. Capillarity ion concentration polarization for spontaneous biomolecular preconcentration mechanism.

    PubMed

    Oh, Yoonjee; Lee, Hyomin; Son, Seok Young; Kim, Sung Jae; Kim, Pilnam

    2016-01-01

    Ionic hydrogel-based ion concentration polarization devices have been demonstrated as platforms to study nanoscale ion transport and to develop engineering applications, such as protein preconcentration and ionic diodes/transistors. Using a microfluidic system composed of a perm-selective hydrogel, we demonstrated a micro/nanofluidic device for the preconcentration of biological samples using a new class of ion concentration polarization mechanism called "capillarity ion concentration polarization" (CICP). Instead of an external electrical voltage source, the capillary force of the perm-selective hydrogel spontaneously generated an ion depletion zone in a microfluidic channel by selectively absorbing counter-ions in a sample solution. We demonstrated a reasonable preconcentration factor (∼100-fold/min) using the CICP device. Although the efficiency was lower than that of conventional electrokinetic ICP operation due to the absence of a drift ion migration, this mechanism was free from the undesirable instability caused by a local amplified electric field inside the ion depletion zone so that the mechanism should be suitable especially for an application where the contents were electrically sensitive. Therefore, this simple system would provide a point-of-care diagnostic device for which the sample volume is limited and a simplified sample handling is demanded.

  10. Capillarity ion concentration polarization for spontaneous biomolecular preconcentration mechanism.

    PubMed

    Oh, Yoonjee; Lee, Hyomin; Son, Seok Young; Kim, Sung Jae; Kim, Pilnam

    2016-01-01

    Ionic hydrogel-based ion concentration polarization devices have been demonstrated as platforms to study nanoscale ion transport and to develop engineering applications, such as protein preconcentration and ionic diodes/transistors. Using a microfluidic system composed of a perm-selective hydrogel, we demonstrated a micro/nanofluidic device for the preconcentration of biological samples using a new class of ion concentration polarization mechanism called "capillarity ion concentration polarization" (CICP). Instead of an external electrical voltage source, the capillary force of the perm-selective hydrogel spontaneously generated an ion depletion zone in a microfluidic channel by selectively absorbing counter-ions in a sample solution. We demonstrated a reasonable preconcentration factor (∼100-fold/min) using the CICP device. Although the efficiency was lower than that of conventional electrokinetic ICP operation due to the absence of a drift ion migration, this mechanism was free from the undesirable instability caused by a local amplified electric field inside the ion depletion zone so that the mechanism should be suitable especially for an application where the contents were electrically sensitive. Therefore, this simple system would provide a point-of-care diagnostic device for which the sample volume is limited and a simplified sample handling is demanded. PMID:26858814

  11. Preconcentration of milk proteins using octadecylated monolithic silica microchip.

    PubMed

    Alzahrani, Eman; Welham, Kevin

    2013-10-10

    Sample preparation is a bottleneck in systems for chemical analysis and it is a required step in order to remove interference and preconcentrate the target analytes. Much research in recent years has focused on porous monolithic materials since they are highly permeable to liquid flow and show high mass transfer compared with common packed beds. This study has focused on the use of a glass microchip containing an inorganic silica-based monolithic material modified with octadecyl groups for preconcentration of milk proteins from skimmed cows' milk that vary in molecular weight, hydrophobicity, and abundance. Comparison between the fabricated device and a commercial cartridge for the preconcentration of proteins in skimmed cows' milk showed the ability of the device to successfully enrich protein mixtures from the sample. The three replicate experiments showed that the RSD of the mass to charge ratio of milk proteins ranged from 0.01 to 0.46%. In addition, it was found that there were no significant differences between the observed and reported masses of the milk proteins and the relative percentage error of the molecular masses ranged between 0.03 and 0.90%. The fact that the small amounts of sample required and short sample preparation time suggest that this new microfluidic device may be a viable alternative to existing procedures for protein extraction from real samples. PMID:24070482

  12. Preconcentration and detection of chlorinated organic compounds and benzene.

    PubMed

    Hobson, Stephen T; Cemalovic, Sabina; Patel, Sanjay V

    2012-03-01

    Remote and automated detection of organic compounds in subsurface aquifers is crucial to superfund monitoring and environmental remediation. Current monitoring techniques use expensive laboratory instruments and trained personnel. The use of a filled tubular preconcentrator combined with a chemicapacitive detector array presents an attractive option for the unattended monitoring of these compounds. Five preconcentrator materials were exposed to common target compounds of subsurface remediation projects (1,1,2-trichloroethane, trichloroethylene, t-1,2-dichloroethylene, benzene, and perchloroethylene). Rapid heating of the tube caused the collected, concentrated effluent to pass over the surface of a chemicapacitive detector array coated with four different sorbent polymers. A system containing a porous ladder polymer and the sensor array was subsequently used to sample the analytes injected onto sand in a laboratory test, simulating a subsurface environment. With extended collection times, effective detection limits of 5 ± 3 ppbV for 1,1,2-trichloroethane and 145 ± 60 ppbV for benzene were achieved. Effects of the preconcentrator material structure, the collection time, and sensor material on the system performance were observed. The resultant system presents a solution for remote, periodic monitoring of chlorinated organic compounds and other volatile organic compounds in a soil matrix.

  13. Determination of Ti, Zr, Nb, V, W and Mo in seawater by a new online-preconcentration method and subsequent ICP-MS analysis

    NASA Astrophysics Data System (ADS)

    Poehle, Sandra; Schmidt, Katja; Koschinsky, Andrea

    2015-04-01

    . The applicability of the on-line preconcentration method was demonstrated for samples collected during a GEOTRACES cruise in the Atlantic. Due to the low limit of quantification, LOQ, and SD, this method enables the determination of ultratrace concentration levels for Ti, Zr, Nb and W as well as the detection of small variations in concentration for all six elements. The required sample volume of only 50 mL, the fast determination within 1 h for all elements and the principle of a closed system are a clear advantage of the analytical procedure compared to many other methods and facilitates sample logistics for the determination of Ti, Zr, Nb, V, W and Mo in seawater. Online-preconcentration method for Ti, Zr, Nb, V, Mo and W in seawater. Detection of ultratrace concentrations for Ti, Zr, Nb and W in seawater. Low standard deviation of the method enables detection of small variations Mo and V. Spikes for Ti, Zr, Nb, V, Mo and W were recovered quantitatively in North Sea water. Quantitative recovery of V and Mo in seawater reference standard NASS-6.

  14. Magnetic materials as sorbents for metal/metalloid preconcentration and/or separation. A review.

    PubMed

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-07-30

    The use of magnetic materials in solid phase extraction has received considerable attention in recent years taking into account many advantages arising from the inherent characteristics of magnetic particles. Magnetic solid phase extraction (MSPE) methodology overcomes problems such as column packing and phase separation, which can be easily performed by applying an external magnetic field. The use of magnetic particles in automatic systems is growing over the last few years making the on-line operation of MSPE a promising technique in the frame of green chemistry. This article aims to provide all recent progress in the research of novel magnetic materials as sorbents for metal preconcentration and determination coupled with different detection systems as well as their implementation in sequential injection and microfluidic systems. In addition, a description of preparation, characterization as well as applications of various types of magnetic materials, either with organic or inorganic coating of the magnetic core, is presented. Concluding remarks and future trends are also commented. PMID:23856225

  15. Microfluidic paper-based biomolecule preconcentrator based on ion concentration polarization.

    PubMed

    Han, Sung Il; Hwang, Kyo Seon; Kwak, Rhokyun; Lee, Jeong Hoon

    2016-06-21

    Microfluidic paper-based analytical devices (μPADs) for molecular detection have great potential in the field of point-of-care diagnostics. Currently, a critical problem being faced by μPADs is improving their detection sensitivity. Various preconcentration processes have been developed, but they still have complicated structures and fabrication processes to integrate into μPADs. To address this issue, we have developed a novel paper-based preconcentrator utilizing ion concentration polarization (ICP) with minimal addition on lateral-flow paper. The cation selective membrane (i.e., Nafion) is patterned on adhesive tape, and this tape is then attached to paper-based channels. When an electric field is applied across the Nafion, ICP is initiated to preconcentrate the biomolecules in the paper channel. Departing from previous paper-based preconcentrators, we maintain steady lateral fluid flow with the separated Nafion layer; as a result, fluorescent dyes and proteins (FITC-albumin and bovine serum albumin) are continuously delivered to the preconcentration zone, achieving high preconcentration performance up to 1000-fold. In addition, we demonstrate that the Nafion-patterned tape can be integrated with various geometries (multiplexed preconcentrator) and platforms (string and polymer microfluidic channel). This work would facilitate integration of various ICP devices, including preconcentrators, pH/concentration modulators, and micro mixers, with steady lateral flows in paper-based platforms. PMID:27199301

  16. Miniaturized Explosive Preconcentrator for Use in a Man-Portable Field Detection System

    SciTech Connect

    Hannum, David W.; Linker, Kevin L.; Parmeter, John E.; Rhykerd, Charles L.; Varley, Nathan R.

    1999-08-02

    We discuss the design and testing of a miniaturized explosives preconcentrator that can be used to enhance the capabilities of man-portable field detection systems, such as those based on ion mobility spectrometry (IMS). The preconcentrator is a smaller version of a similar device that was developed recently at Sandia National Laboratories for use in a trace detection portal that screens personnel for explosives. Like its predecessor, this preconcentrator is basically a filtering device that allows a small amount of explosive residue in a large incoming airflow to be concentrated into a much smaller air volume via adsorption and resorption, prior to delivery into a chemical detector. We discuss laboratory testing of this preconcentrator interfaced to a commercially available IMS-based detection system, with emphasis on the explosives 2,4,6-trinitrotoluene (TNT) and cyclotrimethylenetrinitramine (RDX). The issues investigated include optimization of the preconcentrator volume and inlet airflow, the use of different types of adsorbing surfaces within the preconcentrator, Wd preconcentrator efficiency and concentration factor. We discuss potential field applications of the preconcentrator, as well as avenues for further investigations and improvements.

  17. Sorption preconcentration of vanadium for its determination in sea water

    SciTech Connect

    Andreeva, I.Yu.; Lebedeva, L.I.; Izotova, Yu.A.; Danilova, E.Ya.

    1987-08-10

    This work is devoted to a study of the conditions of vanadium sorption by a fibrous sorbent with a view to evolving a procedure for its determination in sea water. The sorbent was the same as used by them earlier for molybdenum preconcentration. It is a fiber based on polyethylenepolyamine-modified polyacrylonitrile. The sorbent contained 80% tertiary and approx. = 20% primary and secondary amino groups. Static exchange capacity of the sorbent relative to HCl 2 mmole/g, swelling 34%, fiber diameter 0.016 mm. The vanadium content was determined photometrically using acidic chromium blue K.

  18. Progress in metal ion separation and preconcentration : an overview.

    SciTech Connect

    Bond, A. H.

    1998-05-19

    A brief historical perspective covering the most mature chemically-based metal ion separation methods is presented, as is a summary of the recommendations made in the 1987 National Research Council (NRC) report entitled ''Separation and Purification: Critical Needs and Opportunities''. A review of Progress in Metal Ion Separation and Preconcentration shows that advances are occurring in each area of need cited by the NRC. Following an explanation of the objectives and general organization of this book, the contents of each chapter are briefly summarized and some future research opportunities in metal ion separations are presented.

  19. Evaporative preconcentration of fluorescent protein samples in capillary based microplates.

    PubMed

    Shao, Fenfen; Ng, Tuck Wah; Lye, Jonathan Kok Keung; Liew, Oi Wah

    2011-09-01

    The preconcentration of analytes is important in biochemical analysis as it offers the ability to detect for trace species, and increase signal-to-noise ratios when using optical sensing on fluorophores. A strong advantage of the evaporation technique lies in its ability to operate without the need of any energy source; albeit major challenges exist on how to increase the surface area exposure to air for heightened evaporation, ensure no further increases once specified analyte concentrations have been achieved, and not needing any intervening membranes. We demonstrate here that the droplet creation and retraction approach in capillary based microplates offers such abilities whilst at the same time facilitating mixing. PMID:21559858

  20. PNEUMATIC MICROVALVE FOR ELECTROKINETIC SAMPLE PRECONCENTRATION AND CAPILLARY ELECTROPHORESIS INJECTION

    SciTech Connect

    Cong, Yongzheng; Rausch, Sarah J.; Geng, Tao; Jambovane, Sachin R.; Kelly, Ryan T.

    2014-10-27

    Here we show that a closed pneumatic microvalve on a PDMS chip can serve as a semipermeable membrane under an applied potential, enabling current to pass through while blocking the passage of charged analytes. Enrichment of both anionic and cationic species has been demonstrated, and concentration factors of ~70 have been achieved in just 8 s. Once analytes are concentrated, the valve is briefly opened and the sample is hydrodynamically injected onto an integrated microchip or capillary electrophoresis (CE) column. In contrast to existing preconcentration approaches, the membrane-based method described here enables both rapid analyte concentration as well as high resolution separations.

  1. Multiplexed proteomic sample preconcentration device using surface-patterned ion-selective membrane.

    PubMed

    Lee, Jeong Hoon; Song, Yong-Ak; Han, Jongyoon

    2008-04-01

    In this paper, we report a new method of fabricating a high-throughput protein preconcentrator in poly(dimethylsiloxane) (PDMS) microfluidic chip format. We print a submicron thick ion-selective membrane on the glass substrate by using standard patterning techniques. By simply plasma-bonding a PDMS microfluidic device on top of the printed glass substrate, we can integrate the ion-selective membrane into the device and rapidly prototype a PDMS preconcentrator without complicated microfabrication and cumbersome integration processes. The PDMS preconcentrator shows a concentration factor as high as approximately 10(4) in 5 min. This printing method even allows fabricating a parallel array of preconcentrators to increase the concentrated sample volume, which can facilitate an integration of our microfluidic preconcentrator chip as a signal enhancing tool to various detectors such as a mass spectrometer.

  2. Investigation of preconcentration strategies for the trace analysis of multi-residue pesticides in real samples by capillary electrophoresis.

    PubMed

    da Silva, Clóvis L; de Lima, Elizabete C; Tavares, Marina F M

    2003-10-01

    In this work, on-line preconcentration strategies were investigated for the multi-residue analysis of pesticides in drinking water and vegetables using micellar electrokinetic chromatography. Among the on-line strategies, sweeping and stacking with reverse migration of micelles (SRMM), with and without the insertion of a plug of water before sample injection, were contrasted. A new version of SRMM was also introduced. The modification consisted of momentarily applying a positive voltage at the inlet vial right after sample has been injected, increasing the efficiency by which the analytes are captured. Nine pesticides from different classes, carbendazim (benzimidazole), simazine, atrazine, propazine and ametryn (triazine), diuron and linuron (urea), carbaryl and propoxur (carbamate), were baseline separated in less than 6 min with a electrolyte composed of 20 mmol l(-1) phosphate buffer at pH 2.5, containing 25 mmol l(-1) sodium dodecyl sulfate and 10% methanol. Limits of detection (LODs) in the order of 2-46 microg l(-1) for the pesticides under investigation were obtained solely using the on-line strategies. Enrichment factors of 3-18-fold were obtained. These factors were computed as the improvement of the concentration LODs with respect to the reference condition (injection of 10 s at 2.5 kPa pressure). The proposed methodologies were applied to the analysis of pesticides in complex matrices such as carrot extracts where the detection of 2.5 microg l(-1) was illustrated. By combining off-line solid-phase extraction and the proposed on-line strategies, the detection of pesticides in drinking water at the 0.1 microg l(-1) level was conceived. PMID:14558617

  3. On-line atomic data access

    NASA Astrophysics Data System (ADS)

    Schultz, David R.; Nash, Jeffrey K.

    1996-07-01

    The need for atomic data is one which continues to expand in a wide variety of applications including fusion energy, astrophysics, laser-produced plasma research, and plasma processing. Modern computer database and communications technology enables this data to be placed on-line and obtained by users over the INTERNET. Presented here is a summary of the observations and conclusions regarding such on-line atomic data access derived from a forum held at the Tenth APS Topical Conference on Atomic Processes in Plasmas.

  4. Scale Drift in On-Line Calibration.

    ERIC Educational Resources Information Center

    Stocking, Martha L.

    Recent advances in psychometrics and computer technology encourage the development of model-based methods of individualized testing on a microcomputer, where each examinee receives short tests and where the number of pretest items that can be administered is severely restricted. On-line (i.e., data is collected on operational equipment) methods…

  5. LUST ON-LINE CALCULATOR INTRODUCTION

    EPA Science Inventory

    EPA has developed a suite of on-line calculators to assist in performing site assessment and modeling calculations for leaking underground storage tank sites (http://www.epa.gov/athens/onsite). The calculators are divided into four types: parameter estimation, models, scientific...

  6. System and method for preconcentrating, identifying, and quantifying chemical and biological substances

    DOEpatents

    Yu, Conrad M.; Koo, Jackson C.

    2000-01-01

    A system and method for preconcentrating, identifying, and quantifying chemical and biological substances is disclosed. An input valve directs a first volume of a sample gas to a surface acoustic wave (SAW) device. The SAW device preconcentrates and detects a mass of a substance within the sample gas. An output valve receives a second volume of the sample gas containing the preconcentrated substance from the SAW device and directs the second volume to a gas chromatograph (GC). The GC identifies the preconcentrated substance within the sample gas. A shunt valve exhausts a volume of the sample gas equal to the first volume minus the second volume away from the SAW device and the GC. The method of the present invention includes the steps of opening an input valve for passing a first volume of a sample gas to a SAW device; preconcentrating and detecting a mass of a substance within the sample gas using the SAW device; opening an output valve for passing a second volume of the sample gas containing the preconcentrated substance to a gas chromatograph (GC); and then identifying the preconcentrated substance within the sample gas using the GC.

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

    PubMed

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

    2012-02-01

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

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

    PubMed

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

    2012-02-01

    A sensitive and efficient on-line clean up and pre-concentration method has been developed using column-switching technique and protein-coated µ-Bondapak CN silica pre-column for quantification of ambroxol (AM) in human serum. The method is performed by direct injection of serum sample onto a protein-coated µ-Bondapak CN silica pre-column, where AM is pre-concentrated and retained, while proteins and very polar constituents are washed to waste using a phosphate buffer saline (pH 7.4). The retained analyte on the pre-column is directed onto a C(18) analytical column for separation, with a mobile phase consisting of a mixture of methanol and distilled deionized water (containing 1% triethylamine adjusted to pH 3.5 with ortho-phosphoric acid) in the ratio of 50:50 (v/v). Detection is performed at 254 nm. The calibration curve is linear over the concentration range of 12-120 ng/mL (r(2) = 0.9995). The recovery, selectivity, linearity, precision, and accuracy of the method are convenient for pharmacokinetic studies or routine assays. PMID:22298756

  9. Charge state breeders: On-line results

    NASA Astrophysics Data System (ADS)

    Wenander, Fredrik

    2008-10-01

    The transformation of radioactive ions from 1+ to n+ in the low-energy stage of a post-accelerator - also called charge breeding, has become a mature technique. Several machines using the method are in operation or under construction. This paper will present and evaluate on-line and off-line results from two different breeder types, the EBIS and the ECRIS-based systems. Notable on-line results, in terms of versatility, efficiency and beam purity among other things, have been achieved with the trap-EBIS charge breeding system for REX-ISOLDE, a post-accelerator operational since 2001. These will be compared with breeding results of stable and radioactive beams obtained with ECRIS at a number of facilities using or developing ECRIS breeders. Finally an outlook will be given of the predicted evolution of the charge breeders and how they can meet the requirements of future radioactive beam facilities.

  10. On-line controlled documents: Lessons learned

    SciTech Connect

    Cochrell, R.C.; Steele, C.M.

    1995-06-01

    Placing Controlled Documents on-line on a computer network seems like the solution to many problems, one being distribution, with a path toward a paperless office. However, many problems presented themselves as we were designing the system and placing the documents on-line. Although we planned and established a Process Management Team to help work out the bugs, we still encountered many obstacles in the process. This presentation will cover the ``trials and tribulations`` of placing Controlled Documents on a computer network at three different sites. We will discuss the process we went through, the problems we encountered, the software we used, and how we got management to buy into the process.

  11. Trends in on-line data processing

    NASA Astrophysics Data System (ADS)

    Masetti, Massimo

    1981-04-01

    The development of integrated circuits has been characterized by an exponential growth of gates on a single chip that will still continue in the coming years. In parallel the price per bit is dropping down with more or less the same law. As a consequence of this a few statements can be made: -The present 16-bit minicomputer in a small configuration is going to be substituted by a 16-bit microcomputer, and the 16-bit minicomputer in a powerful configuration by a 32-bit midi having also a virtual memory facility. -Fully programmable or microcoded powerful devices like the LASS hardware processor or MICE, will allow an efficient on-line filter. Higher computing-speed can be achieved by a multiprocessor configuration which can be insensitive to hardware failures. Therefore we are moving towards an integrated on-line computing system with much higher computing power than now and the present distinction between on-line and off-line will no longer be so sharp. As more processing can be performed on-line, fast high quality feed-back can be provided for the experiment. In the years to come the trend towards more processing power, at a lower price, and assembled in the same hardware volume will continue for at least five years; at the same time the future large high-energy physics experiments at LEP will be carried out within a wide international collaboration. In this environment methods must be found for a large fraction of the work to be distributed amongst the collaborators. To accomplish this aim it is necessary to introduce common standard practices concerning both hardware and software, in such a way that the separate parts, developed by the collaborators, will be plug-compatible.

  12. Process for separation and preconcentration of radium from water

    DOEpatents

    Dietz, Mark; Horwitz, E. Philip; Chiarizia, Renato; Bartsch, Richard A.

    1999-01-01

    A process for preconcentrating and separating radium from a contaminated solution containing at least water and radium includes the steps of adding a quantity of a water-soluble macrocyclic polyether to the contaminated solution to form a combined solution. An acid is added to the combined solution to form an acidic combined solution having an ›H.sup.+ ! concentration of about 0.5M. The acidic combined solution is contacted with a sulfonic acid-based strong acid cation exchange medium or a organophilic sulfonic acid medium having a plurality of binding sites thereon to bind the radium thereto and to form a radium-depleted solution. The radium-depleted solution is separated from the strong acid cation exchange medium or organophilic sulfonic acid medium. The radium remaining bound to the exchange medium or organophilic reagent is then stripped from the exchange medium or organophilic medium and the activity of the radium is measured.

  13. Process for separation and preconcentration of radium from water

    DOEpatents

    Dietz, M.; Horwitz, E.P.; Chiarizia, R.; Bartsch, R.A.

    1999-01-26

    A process for preconcentrating and separating radium from a contaminated solution containing at least water and radium includes the steps of adding a quantity of a water-soluble macrocyclic polyether to the contaminated solution to form a combined solution. An acid is added to the combined solution to form an acidic combined solution having an [H{sup +}] concentration of about 0.5M. The acidic combined solution is contacted with a sulfonic acid-based strong acid cation exchange medium or a organophilic sulfonic acid medium having a plurality of binding sites thereon to bind the radium thereto and to form a radium-depleted solution. The radium-depleted solution is separated from the strong acid cation exchange medium or organophilic sulfonic acid medium. The radium remaining bound to the exchange medium or organophilic reagent is then stripped from the exchange medium or organophilic medium and the activity of the radium is measured. 24 figs.

  14. Multiplexed electrokinetic sample fractionation, preconcentration and elution for proteomics.

    PubMed

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

    2013-07-01

    Both 6 and 8-channel integrated microfluidic sample pretreatment devices capable of performing "in space" sample fractionation, collection, preconcentration and elution of captured analytes via sheath flow assisted electrokinetic pumping are described. Coatings and monolithic polymer beds were developed for the glass devices to provide cationic surface charge and anodal electroosmotic flow for delivery to an electrospray emitter tip. A mixed cationic ([2-(methacryloyloxy)ethyl] trimethylammonium chloride) (META) and hydrophobic butyl methacrylate-based monolithic porous polymer, photopolymerized in the 6- or 8-fractionation channels, was used to capture and preconcentrate samples. A 0.45 wt% META loaded bed generated comparable anodic electroosmotic flow to the cationic polymer PolyE-323 coated channel segments in the device. The balanced electroosmotic flow allowed stable electrokinetic sheath flow to prevent cross contamination of separated protein fractions, while reducing protein/peptide adsorption on the channel walls. Sequential elution of analytes trapped in the SPE beds revealed that the monolithic columns could be efficiently used to provide sheath flow during elution of analytes, as demonstrated for neutral carboxy SNARF (residual signal, 0.08% RSD, n = 40) and charged fluorescein (residual signal, 2.5% n = 40). Elution from monolithic columns showed reproducible performance with peak area reproducibility of ~8% (n = 6 columns) in a single sequential elution and the run-to-run reproducibility was 2.4-6.7% RSD (n = 4) for elution from the same bed. The demonstrated ability of this device design and operation to elute from multiple fractionation beds into a single exit channel for sample analysis by fluorescence or electrospray mass spectrometry is a crucial component of an integrated fractionation and assay system for proteomics. PMID:23712291

  15. Factors governing the pre-concentration of wastewater using forward osmosis for subsequent resource recovery.

    PubMed

    Ansari, Ashley J; Hai, Faisal I; Guo, Wenshan; Ngo, Hao H; Price, William E; Nghiem, Long D

    2016-10-01

    This study demonstrated a technique using forward osmosis (FO) to pre-concentrate the organic matter in raw wastewater, thereby transforming low strength wastewater into an anaerobically digestible solution. The chemical oxygen demand (COD) of raw wastewater was concentrated up to approximately eightfold at a water recovery of 90%. Thus, even low strength wastewater could be pre-concentrated by FO to the range suitable for biogas production via anaerobic treatment. Excessive salinity accumulation in pre-concentrated wastewater was successfully mitigated by adopting ionic organic draw solutes, namely, sodium acetate, and EDTA-2Na. These two draw solutes are also expected to benefit the digestibility of the pre-concentrated wastewater compared to the commonly used draw solute sodium chloride. Significant membrane fouling was observed when operating at 90% water recovery using raw wastewater. Nevertheless, membrane fouling was reversible and was effectively controlled by optimising the hydrodynamic conditions of the cross-flow FO system. PMID:27236621

  16. High Yield Sample Preconcentration Using a Highly Ion-conductive Charge-selective Polymer

    PubMed Central

    Chun, Honggu; Chung, Taek Dong; Ramsey, J. Michael

    2011-01-01

    The development and analysis of a microfluidic sample preconcentration system using a highly ion-conductive charge-selective polymer (poly-AMPS) is reported. The preconcentration is based on the phenomenon of concentration polarization which develops at the boundaries of the poly-AMPS with buffer solutions. A negatively charged polymer, poly-AMPS, positioned between two microchannels efficiently extracts cations through its large cross section, resulting in efficient anion sample preconcentration. The present work includes the development of a robust polymer that is stable over a wide range of buffers with varying chemical compositions. The sample preconcentration effect remains linear to over 3 mM (0.15 pmol) and 500 μM (15 fmol) for fluorescein and TRITC-tagged albumin solutions, respectively. The system can potentially be used for concentrating proteins on microfluidic devices with subsequent analysis for proteomic applications. PMID:20575520

  17. Recent on-line processing procedures for biological samples for determination of trace elements by atomic spectrometric methods

    NASA Astrophysics Data System (ADS)

    Burguera, José L.; Burguera, Marcela

    2009-06-01

    Few of the elements present in nature play a metabolic role in living organisms. According to their abundance, these elements are classified as macro-, micro- or trace elements, representing 93%, 5% and around 1% respectively, of the total body weight. The remaining percentage could be attributed to those elements with unknown biological functions, to others which are present only because of the exposure to polluted environment or to those intentionally introduced into the body for a special treatment. This review summarizes and discusses the most recent publications related to the on-line processing of biological samples for trace element determination using atomic spectrometry-based detectors. Preconcentration/separation procedures based on solid phase or cloud point extractions, electrochemical deposition, microdialysis, as well as chemical vapor generation are the common practice for improving the sensitivity and selectivity of the available atomic spectrometric techniques. The advantages of using isotope dilution mass spectrometry in speciation studies are also emphasized. Digestion or leaching in oxidizing acidic mixtures aided by heat or by ultrasound or microwave radiation, performed off- or on-line, is necessary to previous steps when processing solid biological samples. The most relevant analytical figures of merit such as detection limits, enrichment factors and sample throughput as well as some aspects related to the on-line system configurations and accuracy assessments are critically presented.

  18. Study of bond Elut® Plexa™ PCX cation exchange resin in flow injection column preconcentration system for metal determination by flame atomic absorption spectrometry.

    PubMed

    Anthemidis, Aristidis N; Xidia, Sofia; Giakisikli, Georgia

    2012-08-15

    A simple and sensitive on-line solid-phase extraction methodology for preconcentration and determination of trace amounts of Cd(II), Pd(II) and Cu(II) in natural water samples has been developed using the strong cation exchange capability of Bond Elut(®) Plexa™ PCX polymer resin. Plexa PCX is a mixed-mode sorbent, commercially available in a cartridge format and as far as we know, there is no application into the field of metal determination. The analytes were retained on the resin, eluted with 1 mol L(-1) hydrochloric acid and subsequently directed to FAAS for quantification. The influence of chemical and flow variables which affect the performance of the system have been studied, providing the appropriate conditions for the analysis of real samples. For preconcentration time of 90 s, an enrichment factor of 90, 95 and 95 and a detection limit (3 s) of 0.1, 1.8 and 0.5 μg L(-1) for Cd(II), Pb(II) and Cu(II), respectively were obtained along with a sampling frequency of 30 h(-1). The accuracy of the proposed method was evaluated by analyzing certified reference materials. This procedure was successfully applied for metal determination in environmental and biological samples. PMID:22841064

  19. Total on-line purchasing system (TOPS)

    SciTech Connect

    Collins, N.

    1995-11-01

    The Information Management Division (IMD) at LLNL is developing a new purchasing system for the Procurement Department. The first major development of this new system is called, {open_quotes}Total On-Line Purchasing System{close_quotes} (TOPS). TOPS will help speed up the requisitioning process by having requisitions electronically entered by requesters and electronically sent to buyers to be put on Purchase Orders. The new purchasing system will use Electronic Commerce (EC)/Electronic Data Interchange (EDI), to help increase transaction flows for shipping notices, RFQs, Quotes, Purchase Orders, and Invoices. ANSI X.12 is the EDI standard that this new EC will use.

  20. On-line consolidation of thermoplastic composites

    NASA Astrophysics Data System (ADS)

    Shih, Po-Jen

    An on-line consolidation system, which includes a computer-controlled filament winding machine and a consolidation head assembly, has been designed and constructed to fabricate composite parts from thermoplastic towpregs. A statistical approach was used to determine the significant processing parameters and their effect on the mechanical and physical properties of composite cylinders fabricated by on-line consolidation. A central composite experimental design was used to select the processing conditions for manufacturing the composite cylinders. The thickness, density, void content, degree of crystallinity and interlaminar shear strength (ILSS) were measured for each composite cylinder. Micrographs showed that complete intimate contact and uniform fiber-matrix distribution were achieved. The degree of crystallinity of the cylinders was found to be in the range of 25-30%. Under optimum processing conditions, an ILSS of 58 MPa and a void content of <1% were achieved for APC-2 (PEEK/Carbon fiber) composite cylinders. An in-situ measurement system which uses a slip ring assembly and a computer data acquisition system was developed to obtain temperature data during winding. Composite cylinders were manufactured with eight K-type thermocouples installed in various locations inside the cylinder. The temperature distribution inside the composite cylinder during winding was measured for different processing conditions. ABAQUS finite element models of the different processes that occur during on-line consolidation were constructed. The first model was used to determine the convective heat transfer coefficient for the hot-air heat source. A convective heat transfer coefficient of 260 w/msp{2°}K was obtained by matching the calculated temperature history to the in-situ measurement data. To predict temperature distribution during winding an ABAQUS winding simulation model was developed. The winding speed was modeled by incrementally moving the convective boundary conditions

  1. Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

    SciTech Connect

    Tan, H.

    1999-03-31

    The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performed in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.

  2. Cloud point extraction preconcentration prior to high-performance liquid chromatography coupled with cold vapor generation atomic fluorescence spectrometry for speciation analysis of mercury in fish samples.

    PubMed

    Yu, Li-Ping

    2005-12-14

    A cloud point extraction methodology was developed for simultaneous preconcentration of Hg(II), methylmercury (MeHg), ethylmercury (EtHg), and phenylmercury (PhHg) prior to reversed-phase high-performance liquid chromatography (HPLC) on-line coupled with cold vapor atomic fluorescence spectrometry for speciation analysis of mercury in fish. The four mercury species were taken into complexes with ammonium pyrrolidine dithiocarbamate (APDC) in aqueous nonionic surfactant Triton X-114 medium and concentrated in the surfactant-rich phase by bringing the solution to the temperature of 40 degrees C. Baseline separation of the enriched complexes was achieved on an RP-C(18) column with a mixture of methanol, acetonitrile, and water (65:15:20, v/v) containing 200 mmol L(-1) HAc (pH 3.5) as the mobile phase. An on-line postcolumn oxidation of the effluent from HPLC, in the presence of K2S2O8 in HCl, was applied in the system followed by an optimal cold vapor generation of mercury species. The variables affecting the complexation and extraction steps were examined. The preconcentration of 10 mL of solution with 0.08% w/v Triton X-114 and 0.04% w/v APDC at pH 3.5 gave enrichment factors of 29, 43, 80, and 98 for MeHg, EtHg, PhHg, and Hg(II), respectively. Low detection limits (S/N = 3) were obtained, ranging from 2 to 9 ng L(-1) (as Hg) for all species. The developed method was successfully applied to the speciation of mercury in real fish samples.

  3. Cloud point extraction preconcentration prior to high-performance liquid chromatography coupled with cold vapor generation atomic fluorescence spectrometry for speciation analysis of mercury in fish samples.

    PubMed

    Yu, Li-Ping

    2005-12-14

    A cloud point extraction methodology was developed for simultaneous preconcentration of Hg(II), methylmercury (MeHg), ethylmercury (EtHg), and phenylmercury (PhHg) prior to reversed-phase high-performance liquid chromatography (HPLC) on-line coupled with cold vapor atomic fluorescence spectrometry for speciation analysis of mercury in fish. The four mercury species were taken into complexes with ammonium pyrrolidine dithiocarbamate (APDC) in aqueous nonionic surfactant Triton X-114 medium and concentrated in the surfactant-rich phase by bringing the solution to the temperature of 40 degrees C. Baseline separation of the enriched complexes was achieved on an RP-C(18) column with a mixture of methanol, acetonitrile, and water (65:15:20, v/v) containing 200 mmol L(-1) HAc (pH 3.5) as the mobile phase. An on-line postcolumn oxidation of the effluent from HPLC, in the presence of K2S2O8 in HCl, was applied in the system followed by an optimal cold vapor generation of mercury species. The variables affecting the complexation and extraction steps were examined. The preconcentration of 10 mL of solution with 0.08% w/v Triton X-114 and 0.04% w/v APDC at pH 3.5 gave enrichment factors of 29, 43, 80, and 98 for MeHg, EtHg, PhHg, and Hg(II), respectively. Low detection limits (S/N = 3) were obtained, ranging from 2 to 9 ng L(-1) (as Hg) for all species. The developed method was successfully applied to the speciation of mercury in real fish samples. PMID:16332112

  4. On-line tritium production monitor

    DOEpatents

    Mihalczo, J.T.

    1993-11-23

    A scintillation optical fiber system for the on-line monitoring of nuclear reactions in an event-by-event manner is described. In the measurement of tritium production one or more optical fibers are coated with enriched {sup 6}Li and connected to standard scintillation counter circuitry. A neutron generated {sup 6}Li(n)T reaction occurs in the coated surface of {sup 6}Li-coated fiber to produce energetic alpha and triton particles one of which enters the optical fiber and scintillates light through the fiber to the counting circuit. The coated optical fibers can be provided with position sensitivity by placing a mirror at the free end of the fibers or by using pulse counting circuits at both ends of the fibers. 5 figures.

  5. On-line tritium production monitor

    DOEpatents

    Mihalczo, John T.

    1993-01-01

    A scintillation optical fiber system for the on-line monitoring of nuclear reactions in an event-by-event manner is described. In the measurement of tritium production one or more optical fibers are coated with enriched .sup.6 Li and connected to standard scintillation counter circuitry. A neutron generated .sup.6 Li(n )T reaction occurs in the coated surface of .sup.6 Li-coated fiber to produce energetic alpha and triton particles one of which enters the optical fiber and scintillates light through the fiber to the counting circuit. The coated optical fibers can be provided with position sensitivity by placing a mirror at the free end of the fibers or by using pulse counting circuits at both ends of the fibers.

  6. On-line process control monitoring system

    DOEpatents

    O'Rourke, Patrick E.; Van Hare, David R.; Prather, William S.

    1992-01-01

    An on-line, fiber-optic based apparatus for monitoring the concentration of a chemical substance at a plurality of locations in a chemical processing system comprises a plurality of probes, each of which is at a different location in the system, a light source, optic fibers for carrying light to and from the probes, a multiplexer for switching light from the source from one probe to the next in series, a diode array spectrophotometer for producing a spectrum from the light received from the probes, and a computer programmed to analyze the spectra so produced. The probes allow the light to pass through the chemical substance so that a portion of the light is absorbed before being returned to the multiplexer. A standard and a reference cell are included for data validation and error checking.

  7. On-line Resources for Xenopus

    PubMed Central

    Bowes, Jeff

    2015-01-01

    Summary Since the advent of computational methods in biology the quantity of biological data has grown exponentially. These data support genomic, genetic, developmental, and other forms of biological experimentation. The number of on-line resources has kept pace with the growth in data. Xenopus has perhaps lagged some of the other model organisms in developing resources but is now quickly catching up. There are now a number of well-established and developing resources for Xenopus. This chapter looks beyond the widely-known public databases, Genbank and the EBI, and describes how the researcher can use a number of central sites such as Xenbase, UniProtKB, and major genome browsers to navigate to a variety of different resources. PMID:22956109

  8. On-line chemical composition analyzer development

    SciTech Connect

    Roberts, M.J.; Garrison, A.A.; Muly, E.C.; Moore, C.F.

    1992-02-01

    The energy consumed in distillation processes in the United States represents nearly three percent of the total national energy consumption. If effective control of distillation columns can be accomplished, it has been estimated that it would result in a reduction in the national energy consumption of 0.3%. Real-time control based on mixture composition could achieve these savings. However, the major distillation processes represent diverse applications and at present there does not exist a proven on-line chemical composition sensor technology which can be used to control these diverse processes in real-time. This report presents a summary of the findings of the second phase of a three phase effort undertaken to develop an on-line real-time measurement and control system utilizing Raman spectroscopy. A prototype instrument system has been constructed utilizing a Perkin Elmer 1700 Spectrometer, a diode pumped YAG laser, two three axis positioning systems, a process sample cell land a personal computer. This system has been successfully tested using industrially supplied process samples to establish its performance. Also, continued application development was undertaken during this Phase of the program using both the spontaneous Raman and Surface-enhanced Raman modes of operation. The study was performed for the US Department of Energy, Office of Industrial Technologies, whose mission is to conduct cost-shared R D for new high-risk, high-payoff industrial energy conservation technologies. Although this document contains references to individual manufacturers and their products, the opinions expressed on the products reported do not necessarily reflect the position of the Department of Energy.

  9. Self nanoprecipitating preconcentrate of tamoxifen citrate for enhanced bioavailability.

    PubMed

    Kapse, Sonali V; Gaikwad, Rajiv V; Samad, Abdul; Devarajan, Padma V

    2012-06-15

    We disclose a self nanoprecipitating preconcentrate (SNP) of tamoxifen citrate (TMX), which forms TMX loaded polymeric nanoparticles, on dilution with aqueous media. SNP comprised TMX, polymer (Kollidon SR) and surfactant/s dissolved in a pharmaceutically acceptable vehicle. Binary surfactant mixtures of Aerosol OT (AOT) with Tween 80 revealed synergistic reduction in surface tension to enable both high entrapment efficiency (EE) and low particle size (PS). Synergism of the surfactants was confirmed by molecular interaction parameter(β(σ)). Combination of AOT and Tween 80 resulted in EE (∼85%) and PS (<250nm). Formation of TMX-KSR nanoparticles in situ was reproducible under most experimental conditions and exhibited pH independent behavior. Dilution volume (>80mL) influenced both PS and EE while dilution temperature influenced only PS. Marginal increase in size was evident at the end of 1h nevertheless was not of concern as TMX SNP exhibited near complete release in 1h. DSC and XRD studies revealed amorphous nature of TMX in nanoparticles. FTIR imaging confirmed uniform distribution of TMX in nanoparticles. ESEM and TEM revealed spherical nanoparticles. Biodistribution studies of (99m)Tc labeled TMX SNP in rats revealed no significant absorption however oral pharmacokinetics revealed enhanced oral bioavailability of TMX (165%) compared to TMX suspension. SNP presents a new in situ approach, for design of drug loaded polymeric nanoparticles. PMID:22414426

  10. Preconcentration Method on Modified Silica Fiber for Chromium Speciation

    PubMed Central

    Chahal, Varinder Kaur; Singh, Raghubir; Malik, Ashok Kumar; Matysik, Frank-Michael; Puri, Jugal Kishore

    2012-01-01

    A new method involving pre-concentration on modified silica fiber is described for the speciation of chromium(III) [Cr(III)] and chromium(VI) [Cr(VI)] in aqueous media. This method is based on the different chelating behavior of Cr(III) and Cr(VI) with morpholine-4-carbodithioate (MDTC). Both complexes are extracted on silica fiber modified by sol-gel technology by using 3-aminopropyltriethoxysilane (APS) as a precursor. All extracted samples are directly injected into an high-performance liquid chromatography injector for the simultaneous determination of Cr(III) and Cr(VI). Cr(VI) forms two different complexes, and Cr(III) forms a single complex with MDTC. Therefore, the concentration of Cr(VI) is determined directly from the peak area obtained at 5.4 min; whereas, the assay of Cr(III) is based on subtracting the peak area of Cr(VI) from the total peak area obtained at 4.3 min. Under the optimized conditions, the limits of detection for Cr(III) and Cr(VI) are found to be 0.7 ng/mL and 0.2 ng/mL, respectively. PMID:22291053

  11. Arsenic speciation in environmental waters by a new specific phosphine modified polymer microsphere preconcentration and HPLC-ICP-MS determination.

    PubMed

    Jia, Xiaoyu; Gong, Dirong; Wang, Jiani; Huang, Fuyi; Duan, Taicheng; Zhang, Xian

    2016-11-01

    A new specific phosphine modified polymer microsphere (PPMs) was designed and used as the core adsorbent to comprehensively enrich both inorganic and organic arsenic species in environmental waters by on line solid-phase extraction (SPE). Avoiding any redox reagent, all the four arsenic species have been quantitatively retained on the home made mini-column with large number of positively charged adsorption groups, and then eluted rapidly (within seconds) with a mixed solution of ammonium nitrate and ammonium dihydrogen phosphate. The trace separation and determination of As(III), DMA, MMA and As(V) species have been simultaneously achieved by high performance liquid chromatography hyphenated to inductively coupled plasma spectrometry (HPLC-ICP-MS) technique. This work has developed a versatile tri-n-butylphosphine functionalized polymer microsphere for an efficient and reliable on-line of simultaneous preconcentration and detection of inorganic and organic arsenic speciation. Under the optimized experimental conditions, the enrichment factors obtained for As(III) and DMA with 25mL sample solution were 28, while for MMA and As(V) reached 30. The low detection limits of 1.2ngL(-1), 0.96ngL(-1), 0.82ngL(-1) and 0.91ngL(-1), with the relative standard deviations (RSDs) of 3.9%, 5.6%, 3.2% and 4.5% were obtained for As(III), DMA, MMA and As(V), respectively. The developed method was validated by analyzing Certified Reference Materials GSBZ 07-3171-2014, promising for routine monitoring of arsenic species in lake water, river water and seawater samples. PMID:27591635

  12. Beyond the Mainstream: New Possibilities for Learning On-Line.

    ERIC Educational Resources Information Center

    Barty, Karin

    2000-01-01

    Discusses on-line learning and whether it will become popular in Australia. Focuses on the availability of on-line courses, interaction in the virtual classroom, the need for direct contact, flexible learning, and learning outcomes. (Author/VWL)

  13. Index Access to On-Line Records: An Operational View.

    ERIC Educational Resources Information Center

    Furlong, Elizebeth J.

    1978-01-01

    Describes operational use of on-line field access, a powerful improvement upon search key access to on-line records and a viable alternative to full key word access; and discusses some of the questions considered at Northwestern University Library during a redesign of the technical services modules of the Northwestern On-Line Intergrated System…

  14. On-Line Learning: One Way to Bring People Together

    ERIC Educational Resources Information Center

    Goff-Kfouri, Carol Ann

    2006-01-01

    The purpose of this study was to demonstrate the benefits of on-line learning for adult learners and to further demystify three common misconceptions concerning on-line learning: students certainly do receive support from their on-line professors, the professor is pro-active rather than passive, and students may be more motivated to learn than in…

  15. A Distributed System for Learning Programming On-Line

    ERIC Educational Resources Information Center

    Verdu, Elena; Regueras, Luisa M.; Verdu, Maria J.; Leal, Jose P.; de Castro, Juan P.; Queiros, Ricardo

    2012-01-01

    Several Web-based on-line judges or on-line programming trainers have been developed in order to allow students to train their programming skills. However, their pedagogical functionalities in the learning of programming have not been clearly defined. EduJudge is a project which aims to integrate the "UVA On-line Judge", an existing on-line…

  16. Different strategies for the preconcentration and separation of parabens by capillary electrophoresis.

    PubMed

    Maijó, Irene; Borrull, Francesc; Aguilar, Carme; Calull, Marta

    2013-02-01

    Several strategies, namely, large volume sample stacking (LVSS), field-amplified sample injection (FASI), sweeping, and in-line SPE-CE, were investigated for the simultaneous separation and preconcentration of a group of parabens. A BGE consisting of 20 mM sodium dihydrogenphosphate (pH 2.28) and 150 mM SDS with 15% ACN was used for the separation and preconcentration of the compounds by sweeping, and a BGE consisting of 30 mM sodium borate (pH 9.5) was used for the separation and preconcentration of the compounds by LVSS, FASI, and in-line SPE-CE. Several factors affecting the preconcentration process were investigated in order to obtain the maximum enhancement of sensitivity. The LODs obtained for parabens were in the range of 18-27, 3-4, 2, and 0.01-0.02 ng/mL, and the sensitivity evaluated in terms of LODs was improved up to 29-, 77-, 120-, and 18,400-fold for sweeping, LVSS, FASI, and in-line SPE-CE, respectively. These preconcentration techniques showed potential as good strategies for focusing parabens. The four methods were validated with standard samples to show the potential of these techniques for future applications in real samples, such as biological and environmental samples.

  17. On-line upgrade of program modules

    NASA Technical Reports Server (NTRS)

    Waldrop, Raymond S.; Volz, Richard A.; Smith, Gary W.; Holzbacher-Valero, A. A.; Goldsack, S. J.

    1993-01-01

    This paper presents a taxonomy of problems that must be solved in order to achieve on-line upgradability of long-lived programs, and presents a solution to the fundamental problems in the taxonomy. The solutions are based upon AdaPT, a set of language extensions designed to aid in the distribution of a single Ada program. AdaPT introduces three major units, the public, the partition, and the node. Publics are primarily used to share type information. Partitions are the basic units of distribution while nodes are used to control the configuration of the program. Nodes and partitions can be created dynamically via the allocator. A node-level routine controls the replacement process. The controlling node creates a new instance of the routine being replaced; the run-time system must ensure that the new instance is the updated one. Once access to the new version has been established, all further calls to the module are redirected to the new version and the caller is informed of the change so that it may make subsequent calls directly. When a module is being upgraded, there is a transition period during which both the old and new versions are present. We require that clients of a potentially replaceable module 'check in' with the controlling node. The controlling node keeps track of the number of clients that have been redirected to the replacement. When all have been redirected, the old version can be deallocated.

  18. Central On-Line Data Directory

    NASA Technical Reports Server (NTRS)

    Thieman, J.

    1986-01-01

    The National Space Science Data Center (NSSDC) Central On-Line Data Directory (CODD), which allows the general scientist remote access to information about data sets available not only at NSSDC, but throughout the scientific community, is discussed. A user may search for data set information within CODD by specifying spacecraft name, experiment name, investigator name, and/or keywords. CODD will include information on atmospheric science data sets contained not only within the PCDS, but also within other data sets that are deemed important. Keywords to be used in locating these data sets are currently being formulated. The main type of keyword to be used for categorization of data sets will be discipline related. The primary discipline keyword for PCDS-type data sets would be ATMOSPHERIC SCIENCE. A good set of subdiscipline keywords is needed under this discipline to subdivide the data sets. A sheet containing a strawman set of subdiscipline keywords was distributed, and a request was made for the knowledgeable scientists to modify or replace the proposed keywords.

  19. On-line subsea multiphase flow measurement

    SciTech Connect

    High, G.; Frantzen, K.H.; Marshall, M.

    1995-12-31

    This paper describes the final detailed design, engineering, and installation phase of a Joint Industry Program to qualify a robust subsea multiphase flowmeter module for long-term installation on a North Sea manifold tie-in. Multiphase subsea production has become a common method of hydrocarbon recovery in all areas of offshore E and P. In the North Sea, many developments are subsea satellites with multiphase well-fluids being comingled prior to processing. The system described meets this challenge by offering a cost effective solution to real-time well monitoring as an alternative to the conventional test separator, removing the need for test lines and shutting in wells for testing. The multiphase instrument allows on-line well fluid analysis, and is also an important tool for reservoir management and field analysis, and provides a means of implementing field allocation metering thereby simplifying small marginal field developments. This project is one of the first subsea multiphase flowmeter installations engineered for long-term subsea service, and designed as an integrated component of the subsea production control system.

  20. DIRECT MERCURY ANALYSIS IN ENVIRONMENTAL SOLIDS BY ICPMS WITH ON-LINE SAMPLE ASHING AND MERCURY PRE-CONCENTRATION USING THE DIRECT MERCURY ANALYZER

    EPA Science Inventory



    A Direct Mercury Analyzer based on sample combustion and mercury concentration by gold amalgamation, followed by atomic absorption determination, was interfaced with a quadrupole and a magnet sector ICPMS. In this paper, we discuss design and operating parameters and eval...

  1. DIRECT MERCURY ANALYSIS IN ENVIRONMENTAL SOLIDS BY ICPMS WITH ON-LINE SAMPLE ASHING AND MERCURY PRECONCENTRATION USING A DIRECT MERCURY ANALYZER

    EPA Science Inventory

    Mercury is a persistent, mobile, and highly toxic pollutant. It's biogeochemistry is probably the most complex of any metal. For these reasons, the U.S. Environmental Protection Agency (EPA), through its Office of Research and Development (ORD), has developed a comprehensive res...

  2. On-line purge and trap gas chromatography for monitoring of trihalomethanes in drinking water distribution systems.

    PubMed

    Brown, Michael A; Miller, Sarah; Emmert, Gary L

    2007-06-01

    A method using an automated on-line purge and trap gas chromatograph with a dry electrolytic conductivity detector (DELCD) has been developed for monitoring four regulated trihalomethanes in drinking water distribution systems. This analyzer samples trihalomethanes from drinking water by pervaporation through a silicone capillary membrane contained within a gas extraction cell (GEC) followed by preconcentration using an adsorbent trap. Trihalomethanes are subsequently desorbed from the trap onto a capillary column, separated and detected. The analyzer operates in real-time, samples directly from the drinking water distribution system and is fully automated. The optimization, operation, and evaluation of the analyzer and method are discussed. Method detection limits (MDL) are less than 1.0 microg L(-1) with acceptable estimates for accuracy, and precision. The results from two on-line monitoring studies in chlorinated and chloraminated distribution systems are presented. The performance of the method is compared directly to United Stated Environmental Protection Agency Method 502.2 and shows a very slight, but acceptable bias.

  3. Condensed Phase Membrane Introduction Mass Spectrometry with Direct Electron Ionization: On-line Measurement of PAHs in Complex Aqueous Samples

    NASA Astrophysics Data System (ADS)

    Termopoli, Veronica; Famiglini, Giorgio; Palma, Pierangela; Cappiello, Achille; Vandergrift, Gregory W.; Krogh, Erik T.; Gill, Chris G.

    2016-02-01

    Polycyclic aromatic hydrocarbons (PAHs) are USEPA regulated priority pollutants. Their low aqueous solubility requires very sensitive analytical methods for their detection, typically involving preconcentration steps. Presented is the first demonstrated `proof of concept' use of condensed phase membrane introduction mass spectrometry (CP-MIMS) coupled with direct liquid electron ionization (DEI) for the direct, on-line measurement of PAHs in aqueous samples. DEI is very well suited for the ionization of PAHs and other nonpolar compounds, and is not significantly influenced by the co-elution of matrix components. Linear calibration data for low ppb levels of aqueous naphthalene, anthracene, and pyrene is demonstrated, with measured detection limits of 4 ppb. Analytical response times (t10%-90% signal rise) ranged from 2.8 min for naphthalene to 4.7 min for pyrene. Both intra- and interday reproducibility has been assessed (<3% and 5% RSD, respectively). Direct measurements of ppb level PAHs spiked in a variety of real, complex environmental sample matrices is examined, including natural waters, sea waters, and a hydrocarbon extraction production waste water sample. For these spiked, complex samples, direct PAH measurement by CP-MIMS-DEI yielded minimal signal suppression from sample matrix effects (81%-104%). We demonstrate the use of this analytical approach to directly monitor real-time changes in aqueous PAH concentrations with potential applications for continuous on-line monitoring strategies and binding/adsorption studies in heterogeneous samples.

  4. Preconcentration and detection of mercury with bioluminescent bioreporter E. coli ARL1.

    PubMed

    Solovyev, Andrey I; Koštejn, Martin; Kuncova, Gabriela; Dostálek, Pavel; Rohovec, Jan; Navrátil, Tomáš

    2015-10-01

    Cell wall envelopes treated with sodium hydroxide and spray-dried were used as mercury sorbents. The sorbent having sorption capacity 17.7 ± 0.1 μmol/g determined was employed for preconcentration of mercury containing 1-10 ng/L. After preconcentration, bioavailable mercury was detected in samples of soil, stream, and tap water via induction of bioluminescence of E. coli ARL1. Iron and manganese at concentrations of tenth microgram per liter interfered bioluminescence detection of mercury. In tap water was detected semiquantitatively 0.127 ± 0.1 nmol/L by the induction of bioluminescence of E. coli ARL1 in medium with tryptone after preconcentration using a method of standard addition.

  5. Cloud point preconcentration of germanium and determination by hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Böyükbayram, A. Elif; Volkan, Mürvet

    2000-07-01

    Cloud point methodology has been successfully employed for the preconcentration of germanium at trace levels from aqueous samples prior to hydride generation flame atomic absorption spectrometry (HGAAS). Germanium was taken into complex with quercetin in aqueous non-ionic surfactant (Triton X-114) medium and concentrated in the surfactant rich phase by bringing the solution to the cloud point temperature (19°C). The preconcentration of only 50 ml of solution with 0.1% Triton X-114 and 2×10 -5 M quercetin at pH 6.4 gives a preconcentration factor of 200. Under these conditions, the detection limit (3 s) and the sensitivity of the cloud-point extraction-HGAAS system were 0.59 and 0.0620 μg l -1, respectively. The extraction efficiency was investigated at low germanium concentrations (10-30 μg l -1) and satisfactory recoveries (93-105%) were obtained.

  6. On-line measurement of pulverized coal

    SciTech Connect

    Earley, D.

    2000-07-01

    Coal-fired electric utilities consistently struggle with attempts to improve overall plant performance by achieving optimum combustion. while many techniques are employed, little has been done to optimize combustion at the individual burners. Distribution of windbox airflow and pulverized coal flow can vary greatly. There has been no effective method to measure coal and air, and the utility industry continues to accept these performance inadequacies. In the age of deregulation and with increasing concerns over emissions, the utility industry continues to search for better methods of fuel and airflow measurement and control. This is especially true with the use of low NO{sub x} burners, which require accurate airflow and fuel balance for optimum reduction of NO{sub x} while simultaneously minimizing unburned carbon. In 1997, a large Utility in Germany tested the use of a new coal flow measuring device which utilizes low frequency microwaves to accurately measure the absolute mass flow in coal pipes. When applied to coal outlets from a pulverizer, this device can accurately measure coal flow distribution form pipe-to-pipe. This device has successfully proven its ability to measure coal flow distribution with no maintenance drift problems. Based on the device's success on one mill, the Utility elected to equip all of the pipes on one boiler at this station. Secondary air (SA) is individually ducted to each burner on this boiler (unlike SA in the US); the plant will control airflow to account for fuel imbalances on-line in an attempt to increase plant efficiency by reducing excess oxygen.

  7. Pre-concentration of trace metals from sea-water for determination by graphite-furnace atomic-absorption spectrometry.

    PubMed

    Sturgeon, R E; Berman, S S; Desaulniers, A; Russell, D S

    1980-02-01

    Determination of Cd, Zn, Pb, Cu, Fe, Mn, Co, Cr and Ni in coastal sea-water by graphite-furnace atomic-absorption spectrometry after preconcentration by solvent extraction and use of a chelating ion-exchange resin is described. Following the extraction of the pyrrolidine-N-carbodithioate and oxinate complexes into methyl isobutyl ketone, the trace metals are further preconcentrated by back-extraction into 1.5M nitric acid. Preconcentration on the chelating resin is effected by a combined column and batch technique, allowing greater preconcentration factors to be obtained. Provided samples are appropriately treated to release non-labile metal species prior to preconcentration, both methods yield comparable analytical results with respect to the mean concentrations determined as well as to mean relative standard deviations. Control and treatment of the analytical blank is also described. PMID:18962623

  8. Development of a portable preconcentrator/ion mobility spectrometer system for the trace detection of narcotics

    SciTech Connect

    Parmeter, J.E.; Custer, C.A.

    1997-08-01

    This project was supported by LDRD funding for the development and preliminary testing of a portable narcotics detection system. The system developed combines a commercial trace detector known as an ion mobility spectrometer (IMS) with a preconcentrator originally designed by Department 5848 for the collection of explosives molecules. The detector and preconcentrator were combined along with all necessary accessories onto a push cart, thus yielding a fully portable detection unit. Preliminary testing with both explosives and narcotics molecules shown that the system is operational, and that it can successfully detect drugs as marijuana, methamphetamine (speed), and cocaine based on their characteristics IMS signatures.

  9. Enhanced preconcentration of selected chlorofluorocarbons on multiwalled carbon nanotubes with polar functionalities.

    PubMed

    Saridara, Chutarat; Hussain, Chaudhery Mustansar; Ragunath, Smruti; Mitra, Somenath

    2015-02-01

    Chromatographic monitoring of chlorofluorocarbons in air requires the preconcentration of these highly volatile species. In this paper, we present functionalized multiwalled carbon nanotubes as effective sorbents for a microtrap designed for chlorofluorocarbons preconcentration. Among the commercial carbons and carbon nanotubes studied, functionalization via carboxylation and propyl amine was most effective for dichlorofluoromethane and trichlorofluoromethane (Freon 11), which were selected as representative chlorofluorocarbons. The results show that carbon nanotubes functionalized with a polar groups led to as much as a 300% increase in breakthrough volume and the desorption bandwidth was reduced by 2.5 times. PMID:25403651

  10. Enhanced preconcentration of selected chlorofluorocarbons on multiwalled carbon nanotubes with polar functionalities.

    PubMed

    Saridara, Chutarat; Hussain, Chaudhery Mustansar; Ragunath, Smruti; Mitra, Somenath

    2015-02-01

    Chromatographic monitoring of chlorofluorocarbons in air requires the preconcentration of these highly volatile species. In this paper, we present functionalized multiwalled carbon nanotubes as effective sorbents for a microtrap designed for chlorofluorocarbons preconcentration. Among the commercial carbons and carbon nanotubes studied, functionalization via carboxylation and propyl amine was most effective for dichlorofluoromethane and trichlorofluoromethane (Freon 11), which were selected as representative chlorofluorocarbons. The results show that carbon nanotubes functionalized with a polar groups led to as much as a 300% increase in breakthrough volume and the desorption bandwidth was reduced by 2.5 times.

  11. EOS ODL Metadata On-line Viewer

    NASA Astrophysics Data System (ADS)

    Yang, J.; Rabi, M.; Bane, B.; Ullman, R.

    2002-12-01

    We have recently developed and deployed an EOS ODL metadata on-line viewer. The EOS ODL metadata viewer is a web server that takes: 1) an EOS metadata file in Object Description Language (ODL), 2) parameters, such as which metadata to view and what style of display to use, and returns an HTML or XML document displaying the requested metadata in the requested style. This tool is developed to address widespread complaints by science community that the EOS Data and Information System (EOSDIS) metadata files in ODL are difficult to read by allowing users to upload and view an ODL metadata file in different styles using a web browser. Users have the selection to view all the metadata or part of the metadata, such as Collection metadata, Granule metadata, or Unsupported Metadata. Choices of display styles include 1) Web: a mouseable display with tabs and turn-down menus, 2) Outline: Formatted and colored text, suitable for printing, 3) Generic: Simple indented text, a direct representation of the underlying ODL metadata, and 4) None: No stylesheet is applied and the XML generated by the converter is returned directly. Not all display styles are implemented for all the metadata choices. For example, Web style is only implemented for Collection and Granule metadata groups with known attribute fields, but not for Unsupported, Other, and All metadata. The overall strategy of the ODL viewer is to transform an ODL metadata file to a viewable HTML in two steps. The first step is to convert the ODL metadata file to an XML using a Java-based parser/translator called ODL2XML. The second step is to transform the XML to an HTML using stylesheets. Both operations are done on the server side. This allows a lot of flexibility in the final result, and is very portable cross-platform. Perl CGI behind the Apache web server is used to run the Java ODL2XML, and then run the results through an XSLT processor. The EOS ODL viewer can be accessed from either a PC or a Mac using Internet

  12. DOE-EPRI On-Line Monitoring Implementation Guidelines

    SciTech Connect

    E. Davis, R. Bickford

    2003-01-02

    Industry and EPRI experience at several plants has shown on-line monitoring to be very effective in identifying out-of-calibration instrument channels or indications of equipment-degradation problems. The EPRI implementation project for on-line monitoring has demonstrated the feasability of on-line monitoring at several participating nuclear plants. The results have been very enouraging, and substantial progress is anticipated in the coming years.

  13. Determination of organic and inorganic mercury species in water and sediment samples by HPLC on-line coupled with ICP-MS.

    PubMed

    dos Santos, José Soares; de la Guárdia, Miguel; Pastor, Augustin; dos Santos, Maria Lúcia Pires

    2009-11-15

    This paper describes a preconcentration method for Hg(2+) and MeHg(+) in water samples using sodium diethyldithiocarbamate immobilized in polyurethane foam (PU-NaDDC) and an extraction method for several mercury species in sediment samples, including MeHg(+), EtHg(+) and PhHg(+), which is simple, rapid, and uses a single organic solvent. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Initially, the test of recovery was applied using procedures compatible with HPLC. Under the optimum extraction conditions, recoveries of 96.7, 96.3 and 97.3% were obtained for MeHg(+), EtHg(+), and PhHg(+), respectively, from n=4 spiked sediment samples. This study also demonstrates that the combination of solid-phase extraction on PU-NaDDC with HPLC separation and ICP-MS detection is an effective preconcentration procedure for simultaneous measurement of Hg(2+) and MeHg(+) at ultra-trace levels in water samples. The application of the proposed procedure to the determination of mercury species in drinking water sample was investigated. The proposed method clearly gave satisfactory average recoveries between 93.7 and 101.5%.

  14. On-line micro-volume introduction system developed for lower density than water extraction solvent and dispersive liquid-liquid microextraction coupled with flame atomic absorption spectrometry.

    PubMed

    Anthemidis, Aristidis N; Mitani, Constantina; Balkatzopoulou, Paschalia; Tzanavaras, Paraskevas D

    2012-07-01

    A simple and fast preconcentration/separation dispersive liquid-liquid micro extraction (DLLME) method for metal determination based on the use of extraction solvent with lower density than water has been developed. For this purpose a novel micro-volume introduction system was developed enabling the on-line injection of the organic solvent into flame atomic absorption spectrometry (FAAS). The effectiveness and efficiency of the proposed system were demonstrated for lead and copper preconcentration in environmental water samples using di-isobutyl ketone (DBIK) as extraction solvent. Under the optimum conditions the enhancement factor for lead and copper was 187 and 310 respectively. For a sample volume of 10 mL, the detection limit (3 s) and the relative standard deviation were 1.2 μg L(-1) and 3.3% for lead and 0.12 μg L(-1) and 2.9% for copper respectively. The developed method was evaluated by analyzing certified reference material and it was applied successfully to the analysis of environmental water samples.

  15. Specific-lon electrode determinations of sulfide preconcentrated from San Francisco Bay waters

    USGS Publications Warehouse

    Vivit, D.V.; Ball, J.W.; Jenne, E.A.

    1984-01-01

    Measurements of low-level dissolved-sulfide concentrations in estuarine water from San Francisco Bay have been made using the sulfide-specific electrode after preservation, separation, and preconcentration of the sulfide species. The separation and preconcentration were acheived by coprecipitation of ZnS with Zn(OH)2 followed by collection and dissolution of the precipitate, giving concentration factors up to 160-fold Preconcentration provided sulfide solutions that were adequately measurable within the practical working range of the specific-ion electrode The sulfide detection limit with the preconcentration step is 0 02 ??g/l Spike recoveries in the range of 81 to 10 1% have been achieved for laboratory-prepared samples having S2- concentrations as low as 0 6 ??g/l and 84 to 100% for an estuarine sample spiked in the field with 2 ??g/l (S(-II) Positive correlations have been found between dissolved S(-II) concentrations and concentrations of dissolved Cd, Cu, and Ni, negative correlations have been found between bisulfide (HS-) activity and activities of Cd2+, Cu2+, and Ag+ species ?? 1984 Springer-Verlag New York Inc.

  16. Real-time dual-loop electric current measurement for label-free nanofluidic preconcentration chip.

    PubMed

    Chung, Pei-Shan; Fan, Yu-Jui; Sheen, Horn-Jiunn; Tian, Wei-Cheng

    2015-01-01

    An electrokinetic trapping (EKT)-based nanofluidic preconcentration device with the capability of label-free monitoring trapped biomolecules through real-time dual-loop electric current measurement was demonstrated. Universal current-voltage (I-V) curves of EKT-based preconcentration devices, consisting of two microchannels connected by ion-selective channels, are presented for functional validation and optimal operation; universal onset current curves indicating the appearance of the EKT mechanism serve as a confirmation of the concentrating action. The EKT mechanism and the dissimilarity in the current curves related to the volume flow rate (Q), diffusion coefficient (D), and diffusion layer (DL) thickness were explained by a control volume model with a five-stage preconcentration process. Different behaviors of the trapped molecular plug were categorized based on four modes associated with different degrees of electroosmotic instability (EOI). A label-free approach to preconcentrating (bio)molecules and monitoring the multibehavior molecular plug was demonstrated through real-time electric current monitoring, rather than through the use of microscope images.

  17. PRECONCENTRATION OF ALIPHATIC AMINES FROM WATER DETERMINED BY CAPILLARY ELECTROPHORESIS WITH INDIRECT UV DETECTION

    EPA Science Inventory

    Preconcentration methodology based on adsorption chromatographies for enriching aliphatic amines (c1 to C4 substituted primary, secondary, and tertiary) and alkanolamines in water was studied by free zone capillary electrophoresis (CZE)with indirect UV detection. The solid-phase ...

  18. Effect of thermal desorption kinetics on vapor injection peak irregularities by a microscale gas chromatography preconcentrator.

    PubMed

    Seo, Jung Hwan; Liu, Jing; Fan, Xudong; Kurabayashi, Katsuo

    2012-08-01

    Microscale gas chromatography (μGC) is an emerging analytical technique for in situ analysis and on-site monitoring of volatile organic compounds (VOCs) in moderately complex mixtures. One of the critical subcomponents in a μGC system is a microfabricated preconcentrator (μ-preconcentrator), which enables detection of compounds existing in indoor/ambient air at low (~sub ppb) concentrations by enhancing their signals. The prevailing notion is that elution peak broadening and tailing phenomena resulting from undesirable conditions of a microfabricated separation column (μ-column) are the primary sources of poor chromatographic resolution. However, previous experimental results indicate that the resolution degradation still remains observed for a μ-column integrated with other μGC subcomponents even after setting optimal separation conditions. In this work, we obtain the evidence that the unoptimized μ-preconcentrator vapor release/injection performance significantly contributes to decrease the fidelity of μGC analysis using our state-of-the-art passive preconcentrator microdevice. The vapor release/injection performance is highly affected by the kinetics of the thermal desorption of compounds trapped in the microdevice. Decreasing the heating rate by 20% from the optimal rate of 90 °Cs(-1) causes a 340% increase in peak tailing as well as 70% peak broadening (30% peak height reduction) to the microscale vapor injection process.

  19. On-line electrochemically controlled solid-phase extraction interfaced to electrospray and inductively coupled plasma mass spectrometry.

    PubMed

    Liljegren, Gustav; Forsgard, Niklas; Zettersten, Camilla; Pettersson, Jean; Svedberg, Malin; Herranen, Merja; Nyholm, Leif

    2005-10-01

    Electrochemically controlled solid-phase extractions of anions were interfaced on-line to electrospray mass spectrometry (ESI-MS) and inductively coupled plasma mass spectrometry (ICP-MS), using polypyrrole coated electrodes and a thin-layer electrochemical (EC) flow cell. The results indicate that electrochemically controlled solid-phase extraction (EC-SPE) can be used as a versatile potential controlled sample preparation technique for a range of anions and that the properties of the polypyrrole coatings can be modified by altering the electrodeposition conditions. In the present study, the influence of interfering anions (i.e., fluoride and sulfate), and the anion used during the electropolymerisation, on the bromide extraction recovery was investigated for EC-SPE interfaced to ICP-MS. The results of these experiments show that the interference due to the presence of similar concentrations of sulfate can be reduced when using a polypyrrole coating electropolymerised in the presence of bromide ions. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) measurements were also used to study the morphology of the coatings, as well as the variations in the film thickness within the coatings. The effect of different desorption techniques on the bromide preconcentration factor in the ICP-MS on-line flow system was also examined. Stopped-flow desorption was found to give rise to significantly increased preconcentration factors in comparison with desorptions in flowing solutions. While the desorption efficiency depends on the type of desorption electrolyte (the electrolyte in which the desorption takes place), due to the competing influx of cations, the influence of the pH on the switching charge of the polypyrrole coating was found to be small, at constant ionic strength. To study the applicability of the EC-SPE technique with respect to real samples, investigations were also made with tap water samples spiked with different bromide concentrations. The

  20. System Requirements for On-Line and Batch Retrieval.

    ERIC Educational Resources Information Center

    American Society for Information Science, Washington, DC. Special Interest Group on Computerized Retrieval Services.

    Three papers on system requirements for on-line and batch retrieval presented at the American Society for Information Science (ASIS) annual meeting are included here. At G.D. Searle, data for records related to pharmacology screening are used in a batch system, and an on-line system is used to search information on mutagenic, carcinogenic, and…

  1. 45 CFR 502.8 - Documents on-line.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 45 Public Welfare 3 2011-10-01 2011-10-01 false Documents on-line. 502.8 Section 502.8 Public Welfare Regulations Relating to Public Welfare (Continued) FOREIGN CLAIMS SETTLEMENT COMMISSION OF THE... § 502.8 Documents on-line. Commission documents available in electronic format may be accessed via...

  2. 45 CFR 502.8 - Documents on-line.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 45 Public Welfare 3 2010-10-01 2010-10-01 false Documents on-line. 502.8 Section 502.8 Public Welfare Regulations Relating to Public Welfare (Continued) FOREIGN CLAIMS SETTLEMENT COMMISSION OF THE... § 502.8 Documents on-line. Commission documents available in electronic format may be accessed via...

  3. Evidence on the Effectiveness of On-Line Homework

    ERIC Educational Resources Information Center

    Dillard-Eggers, Jane; Wooten, Tommy; Childs, Brad; Coker, John

    2008-01-01

    The purpose of this research is to evaluate the impact and effectiveness of on-line homework in principles of accounting classes. We surveyed students to determine their degree of satisfaction with on-line homework and their perceptions about its effectiveness in enhancing their learning. We also gathered data to determine the extent of online…

  4. On-Line Library Housekeeping Systems. A Survey

    ERIC Educational Resources Information Center

    McAllister, Caryl

    1971-01-01

    A general discussion of on-line procedures, batch and real-time updating, types of files and indexes, terminals, and the use of a general-purpose data management system as a vehicle for on-line operation is followed by an Appendix giving detailed information on each on the known systems. (14 references) (Author/NH)

  5. Are On-Line Data Bases in Your Library's Future?

    ERIC Educational Resources Information Center

    Deacon, Jim

    1983-01-01

    THE FOLLOWING IS THE FULL TEXT OF THIS DOCUMENT: Today there are over 900 on-line data banks available for public access. Most microcomputers can use them through the aid of a modem and communication program. Major public information utilities that offer access to these on-line data bases are growing and expanding. The Source, a data base utility…

  6. On-Line Course Development: Engaging and Retaining Students

    ERIC Educational Resources Information Center

    Bruster, Benita G.

    2015-01-01

    As the number of on-line classes and the demand for on-line education continues to sky-rocket, it is critical that course developers and university faculty have the skills to effectively design curricula, to develop engaging learning opportunities, and to create responsive courses that meet individual student needs. This paper details three…

  7. On-Line and Off-Line Assessment of Metacognition

    ERIC Educational Resources Information Center

    Saraç, Seda; Karakelle, Sema

    2012-01-01

    The study investigates the interrelationships between different on-line and off-line measures for assessing metacognition. The participants were 47 fifth grade elementary students. Metacognition was assessed through two off-line and two on-line measures. The off-line measures consisted of a teacher rating scale and a self-report questionnaire. The…

  8. Determination of cadmium in alcohol fuel using Moringa oleifera seeds as a biosorbent in an on-line system coupled to FAAS.

    PubMed

    Alves, Vanessa Nunes; Mosquetta, Rafael; Coelho, Nívia Maria Melo; Bianchin, Joyce Nunes; Di Pietro Roux, Kalya Cravo; Martendal, Edmar; Carasek, Eduardo

    2010-01-15

    In this study a new method for determination of cadmium in alcohol fuel using Moringa oleifera seeds as a biosorbent in an on-line preconcentration system coupled to flame atomic absorption spectrometry (FAAS) was developed. Flow and chemical variables of the proposed system were optimized through multivariate designs. The limit of detection for cadmium was 5.50microg L(-1) and the precision was below 2.3% (35.0microg L(-1), n=9). The analytical curve was linear from 5 to 150microg L(-1), with a correlation coefficient of 0.9993. The developed method was successfully applied to spiked alcohol fuel, and accuracy was assessed through recovery tests, with recovery ranging from 97.50 to 100%. PMID:20006064

  9. MSFIA-LOV system for (226)Ra isolation and pre-concentration from water samples previous radiometric detection.

    PubMed

    Rodríguez, Rogelio; Borràs, Antoni; Leal, Luz; Cerdà, Víctor; Ferrer, Laura

    2016-03-10

    An automatic system based on multisyringe flow injection analysis (MSFIA) and lab-on-valve (LOV) flow techniques for separation and pre-concentration of (226)Ra from drinking and natural water samples has been developed. The analytical protocol combines two different procedures: the Ra adsorption on MnO2 and the BaSO4 co-precipitation, achieving more selectivity especially in water samples with low radium levels. Radium is adsorbed on MnO2 deposited on macroporous of bead cellulose. Then, it is eluted with hydroxylamine to transform insoluble MnO2 to soluble Mn(II) thus freeing Ra, which is then coprecipitated with BaSO4. The (226)Ra can be directly detected in off-line mode using a low background proportional counter (LBPC) or through a liquid scintillation counter (LSC), after performing an on-line coprecipitate dissolution. Thus, the versatility of the proposed system allows the selection of the radiometric detection technique depending on the detector availability or the required response efficiency (sample number vs. response time and limit of detection). The MSFIA-LOV system improves the precision (1.7% RSD), and the extraction frequency (up to 3 h(-1)). Besides, it has been satisfactorily applied to different types of water matrices (tap, mineral, well and sea water). The (226)Ra minimum detectable activities (LSC: 0.004 Bq L(-1); LBPC: 0.02 Bq L(-1)) attained by this system allow to reach the guidance values proposed by the relevant international agencies e.g. WHO, EPA and EC. PMID:26893088

  10. Evaluation and optimization of an on-line admicelle-based extraction-liquid chromatography approach for the analysis of ionic organic compounds.

    PubMed

    Merino, Francisco; Rubio, Soledad; Pérez-Bendito, Dolores

    2004-07-15

    Admicelles-based solid-phase extraction (SPE) was on-line coupled with liquid chromatography/electrospray ionization/ion trap mass spectrometry, and it was proposed for the extraction of ionic organic compounds based on the formation of surfactant-analyte ion pairs. The approach was illustrated by studying the preconcentration of quaternary ammonium herbicides (quats) on sodium dodecyl sulfate (SDS) admicelles produced on alumina. Optimization of the parameters affecting SPE were studied on the basis that admicelles are dynamic entities in equilibrium with the aqueous phase. Some general guidelines could be established for method development from the results obtained. Factors influencing on-line operation were elucidated. On-line regeneration of the sorbent in each run was easily achieved by disruption of SDS admicelles with methanol and posterior coating of the alumina with SDS. The recovery of quats from drinking water samples were found quantitative for paraquat, diquat, and difenzoquat and above to 70% for chlormequat and mepiquat. Concentration factors of about 250, using sample volumes of 50 mL, were achieved. The detection limits ranged from 10 to 30 ng/L. The approach developed permits compliance with the directives of the European Community for drinking waters (100 ng/L) and goes deeply into the basis of solid-phase extractions that use surfactant-coated mineral oxide as sorbents.

  11. MULTIELEMENT SOLID PHASE PRECONCENTRATION USING A CHELATING RESIN OF STYRENE DIVINYLBENZENE COPOLYMER AND APPLICATION TO ANALYSIS OF SEAWATER AND FISH OTOLITHS BY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (ICP�MS)

    PubMed Central

    Zereen, Fahmida; Yilmaz, Vedat; Arslan, Zikri

    2013-01-01

    A new chelating resin has been synthesized by immobilizing 4–(2–thiazolylazo) resorcinol (TAR) onto styrene divinlybenzene copolymer and examined for on-line solid phase extraction/preconcentration of Cd, Co, Cu, Ni, Pb and Zn in seawater and fish otoliths for determination by inductively plasma mass spectrometry (ICP-MS). A volume of 5.0 mL sample solution was loaded onto the mini column of TAR immobilized resin at 2.0 mL min−1 via a sequential injection system. The optimum pH for multielement preconcentration was around pH 5.5. Recoveries were better than 96% in artificial seawater. Elution was achieved with 1.0 mL of 0.75 mol L−1 HNO3. The resin possesses large sorption capacity ranging from 82.0 µmol g−1 for Pb to 319 µmol g−1 for Cu. The detection limits (3s) varied between 0.0016 µg L−1 (Cd) and to 0.015 µg L−1 (Zn) for preconcentration of 5.0 mL blank solutions (pH 5.5). Relative standard deviation (RSD)for three replicate runs was between 0.3% (Cd) and 6% (Zn) at 1.0 µg L−1 level. The procedure was validated by analysis of Nearshore Seawater certified reference material (CASS–4), and then successfully applied to the determination of the trace elements in fish otoliths (CRM 22) and in coastal seawater and estuarine water samples. PMID:24976635

  12. An on-line stacking capillary electrophoresis method for the analysis of Δ(9)-tetrahydrocannabinol and its metabolites.

    PubMed

    Cheng, Hui-Ling; Tsai, Yi-Hsuan; Hsu, Wan-Ling; Lin, Yi-Hui

    2015-12-24

    The objective of this study was to establish a practical and reliable analytical method for monitoring trace amounts of Δ(9)-tetrahydrocannabinol (THC) and its metabolites in biological samples. A novel on-line preconcentration capillary electrophoresis method combining large volume sample injection, anion selective exhaustive injection and sweeping was developed to enhance analytical sensitivity. A background buffer composed with 30mM phosphate buffer (pH 2.5) containing 40% methanol and 100mM SDS was used to suppress the electroosmotic flow of the uncoated fused silica capillary (40cm×50μm i.d.). High conductivity buffer (200mM phosphate, pH 2.5) was injected for analyte accumulation. The samples, prepared in phosphate buffer or Tris buffer, were introduced by hydrodynamic injection and electrokinetic injection. After sweeping, the separation was performed in micellar electrokinetic chromatography (MEKC) mode at -15kV. During the method validation, the coefficient of determination of the regression curve was measured at greater than 0.993, and the relative standard deviation and relative error were lower than 11.06% and 9.24%, respectively. Under optimized conditions, an improvement of up to 2000-fold higher sensitivity was achieved. This method was applied to the analysis of urine samples, indicating that it could be satisfactorily utilized in the toxicological and clinical monitoring of cannabis. PMID:26643722

  13. Preparing Students for Assessment in the On-Line Class.

    ERIC Educational Resources Information Center

    Ford, Michele L.

    2002-01-01

    Advises professors with limited technological experience on how to use features of their existing computer networks to communicate assessment expectations to their on-line students. Explains how e-mail and Web postings can serve this purpose. (EV)

  14. Microwave acid digestion and preconcentration neutron activation analysis of biological and diet samples for iodine.

    PubMed

    Rao, R R; Chatt, A

    1991-07-01

    A simple preconcentration neutron activation analysis (PNAA) method has been developed for the determination of low levels of iodine in biological and nutritional materials. The method involves dissolution of the samples by microwave digestion in the presence of acids in closed Teflon bombs and preconcentration of total iodine, after reduction to iodide with hydrazine sulfate, by coprecipitation with bismuth sulfide. The effects of different factors such as acidity, time for complete precipitation, and concentrations of bismuth, sulfide, and diverse ions on the quantitative recovery of iodide have been studied. The absolute detection limit of the PNAA method is 5 ng of iodine. Precision of measurement, expressed in terms of relative standard deviation, is about 5% at 100 ppb and 10% at 20 ppb levels of iodine. The PNAA method has been applied to several biological reference materials and total diet samples. PMID:1897721

  15. Anion separation and preconcentration with cyclen and cyclen-resorcinarene derivatives.

    PubMed

    Wang, Jing; Harrison, Roger G; Lamb, John D

    2009-08-01

    N-undecyl cyclen and a resorcinarene bowl bearing four cyclen arms have been applied as anion exchangers in ion chromatography by strong adsorption to a reversed-phase column. The column loaded with the resorcinarene bowl cyclen tetramer exhibited significantly better performance in anion separation than that with N-undecyl cyclen monomer in isocratic elution mode. Both columns were tested for polarizable anion preconcentration or removal. By changing the eluent type from sodium bicarbonate to sodium hydroxide, the degree of protonation of the cyclen molecules could be modified, and the column capacity for anion retention adjusted thereby. Capacity gradient elution was successfully applied to removing sample matrix ions in the preconcentration of perchlorate and perrhenate ions as example analytes. PMID:19772718

  16. Microwave acid digestion and preconcentration neutron activation analysis of biological and diet samples for iodine.

    PubMed

    Rao, R R; Chatt, A

    1991-07-01

    A simple preconcentration neutron activation analysis (PNAA) method has been developed for the determination of low levels of iodine in biological and nutritional materials. The method involves dissolution of the samples by microwave digestion in the presence of acids in closed Teflon bombs and preconcentration of total iodine, after reduction to iodide with hydrazine sulfate, by coprecipitation with bismuth sulfide. The effects of different factors such as acidity, time for complete precipitation, and concentrations of bismuth, sulfide, and diverse ions on the quantitative recovery of iodide have been studied. The absolute detection limit of the PNAA method is 5 ng of iodine. Precision of measurement, expressed in terms of relative standard deviation, is about 5% at 100 ppb and 10% at 20 ppb levels of iodine. The PNAA method has been applied to several biological reference materials and total diet samples.

  17. Capillary electrochromatography and preconcentration of neutral compounds on poly(dimethylsiloxane) microchips.

    PubMed

    Ro, Kyung Won; Chang, Woo-Jin; Kim, Ho; Koo, Yoon-Mo; Hahn, Jong Hoon

    2003-09-01

    Capillary electrochromatography (CEC) and preconcentration of neutral compounds have been realized on poly(dimethylsiloxane) (PDMS) microchips. The channels are coated with polyelectrolyte multilayers to avoid absorption of hydrophobic analytes into PDMS. The structures of a microchip include an injector and a bead chamber with integrated frits, where the particles of the stationary phase are completely retained. Dimensions of the frit structures are 25 micro mx20 micro m, and the space between the structures is 3 micro m. A neutral compound, BODIPY, that is strongly absorbed into native PDMS, is successfully and selectively retained on octadecylsilane-coated silica beads in the bead chamber with a concentration enhancement of up to 100 times and eluted with elution buffer solution containing 70% acetonitrile. Preconcentrations and CEC separations of coumarins have been conducted with the same device and achieved complete separations in less than 50 s. PMID:14518053

  18. Preconcentration of trace metals from sea water with 7-dodecenyl-8-quinolinol impregnated macroporous resin

    SciTech Connect

    Isshiki, K.; Tsuji, F.; Kuwamoto, T.; Nakayama, E.

    1987-10-15

    7-Dodecenyl-8-quinolinol (DDQ) impregnated XAD-4 resin (DDQ resin) was prepared, and its extraction behavior was studied and compared with solvent extraction with DDQ for Aq, Al, Bi, Cd, Cu, Fe, Ga, Mn, Ni, Pb, and Ti. The results demonstrate that the DDQ resin is effective in the preconcentration of those metals from sea water. The column extraction method using the DDQ resin was applied to sea water analysis with satisfactory results being obtained.

  19. Preconcentration of Aromatic Compounds in Aqueous Samples with a Polymer-coated Fiber-packed Capillary and Subsequent Temperature-programmed Elution with Water for Pseudo-2D LC Separations.

    PubMed

    Tazawa, Toshiaki; Mori, Yuuhi; Kobayashi, Akira; Nakane, Kenichi; Monobe, Tomoya; Ueta, Ikuo; Saito, Yoshihiro

    2015-01-01

    A bundle of polymer-coated filaments was successfully introduced as an extraction medium for the preconcentration of an aqueous solution of aromatic compounds. The extraction was simply carried out with pumping the aqueous sample solution to the extraction capillary at ambient temperature. The extracted analytes were sequentially eluted with a flow of pure water using temperature-programmed heating of the extraction capillary in an oven. The results clearly suggest that the polymer-coated fiber-packed capillary could be employed in the sample preparation process for the analysis of various aqueous samples. Introducing the fractions eluted from the fiber-packed capillary to a conventional microcolumn liquid chromatography (micro-LC) system via a home-made valve-based modulator, an on-line coupled extraction/separation system was developed and a possibility to a pseudo-two-dimensional (pseudo-2D) LC separation of aromatic compounds in aqueous matrices has also been demonstrated.

  20. Multiple capillary isotachophoresis with repetitive hydrodynamic injections for performance improvement of the electromigration preconcentration.

    PubMed

    Mai, Thanh Duc; Oukacine, Farid; Taverna, Myriam

    2016-07-01

    A novel electrokinetic preconcentration technique based on multiple isotachophoresis (M-ITP) realised in a micro-bored capillary to improve sensitivity for capillary electrophoresis with hydrodynamic injection was developed. The M-ITP operation relies on pressure-assisted pushing of a preconcentrated sample plug after the first ITP process back to the injection end of the capillary, followed by a large volume hydrodynamic injection prior to application of the second ITP step. This operational cycle was repeated as many times as desired with very good repeatability of the peak areas and peak heights at each ITP round (RSD less than 8%). Using imidazole and benzoate as models for cationic and anionic analytes, important insights into the mechanism of this electrokinetic preconcentration process with and without the presence of the electro-osmotic flow (EOF) at acidic and basic conditions were provided. Stacking of the benzoate ion, selected as one model analyte, in the presence of EOF and from a sample plug representing up to 300% of the total capillary length was successfully demonstrated. M-ITP was then demonstrated through the enrichment of the Aβ 1-40 amyloid peptide, considered as one of the biomarkers for biochemical diagnosis of Alzheimer's disease. Quantification of Aβ 1-40 down to 50nM with UV detection was made possible with 6 M-ITP cycles. PMID:27236482

  1. Integration of nanoporous membranes into microfluidic devices: electrokinetic bio-sample pre-concentration.

    PubMed

    Kim, Minseok; Kim, Taesung

    2013-10-21

    The integration of nanoporous membranes into microfluidic devices allows a wide range of analytical and biochemical applications such as stable concentration gradient generation, sample pre-concentration, and ion and biomolecule filtration in a controllable manner. However, further applications of nanoporous membranes in microfluidic devices require rapid and controllable fabrication methods of various nanoporous precursor materials; currently, few such methods exist. Here, we describe simple and robust methods that can be used for microfabricating four different precursor materials as leakage-tight membranes in a microfluidic channel network. The methods consist of a common integration process and individual solidification processes such as solvent evaporation, UV-curing, and temperature treatment. We demonstrate that the fabricated membranes can be used for electrokinetic, nanofluidic pre-concentration of bio-samples such as proteins, cells, and microspheres on either the anodic or cathodic side of the membranes. In addition, we not only characterize the physicochemical properties of the membranes such as conductance of membrane-integrated microchannels, relative permselectivity, and pre-concentration ability, but also compare fabrication availability, membrane robustness, surface charge density tunability and biocompatibility with buffer solutions. The methods are versatile for many nanoporous precursor materials and easy to control the location and dimension of the membranes. Hence, the methods developed and the characterized properties of the membranes tested in this work could be widely employed for further applications of nanoporous membranes in microfluidic systems.

  2. Connecting to On-line Data, a Progress Report

    NASA Astrophysics Data System (ADS)

    Eichhorn, G.; Astrophysics Datacenter Executive Committee (ADEC)

    2004-12-01

    The Astrophysics Datacenter Executive Committee (ADEC) has worked with the American Astronomical Society (AAS) and the University of Chicago Press (UChP) to implement links from the on-line literature to on-line data and vice versa. A first demonstration of this system is on-line in the Astrophysical Journal Supplement, Volume 154, Issue 1, a special issue about first results from Spitzer. Several of these on-line articles have links to on-line data. This linking system requires the collaboration of the data centers (marking data sets with unique identifiers, providing a verification system for identifiers, providing a systematic linking system to data sets), the ADS (providing a master verifier that connects the journal to the individual verifiers at the data centers, providing a linking server that allows stable links for the journals even if data sets move), and the AAS and the UChP (implementing LaTeX tags for identifiers, processing and verifying identifiers, implementing the links). Once the links are in place at the journal website, the publisher returns this information to the ADS and from there to the data centers in order to provide the data centers the information necessary to implement the opposite links from data sets to journal articles. The pipeline for this information flow is now fully in place and will be described in this poster. This work is supported by NASA under sevreal grants.

  3. UNISOR on-line nuclear orientation facility (UNISOR/NOF)

    SciTech Connect

    Girit, I.C.; Alton, G.D.; Bingham, C.R.; Carter, H.K.; Simpson, M.L.; Cole, J.D.; Croft, W.L.; Hamilton, J.H.; Jones, E.F.; Gore, P.M.

    1988-01-01

    The UNISOR on-line nuclear orientation facility (UNISOR/NOF) consists of a /sup 3/He--/sup 4/He dilution refrigerator on line to the isotope separator. Nuclei are implanted directly into a target foil which is soldered to the bottom accessed cold finger of the refrigerator. A 1.5 T superconducting magnet polarizes the ferromagnetic target foils and determines the axis of symmetry. Up to eight gamma detectors can be positioned around the refrigerator, each 9 cm from the target. A unique feature of this system is that the k = 4 term in the directional distribution function can be directly and unambiguously deduced so that a single solution for the mixing ratio can be found. The first on-line experiment at this facility reported here was a study of the decay of the /sup 191/Hg and /sup 193/Hg isotopes. 5 refs., 4 figs., 1 tab.

  4. An on-line NMR technique with a programmable processor

    SciTech Connect

    Razazian, K.; Dieckman, S.L.; Raptis, A.C.

    1995-07-01

    Nuclear magnetic resonance (NMR) spectroscopy is used to determine molecular content of materials, mainly in laboratory measurements. The reduced cost of fast computer processors, together with recent break throughs in digital signal processor technology, has facilitated the on-line use of NMR by allowing modifications of the available technology. This paper describes a system and an algorithm for improving the on-line operations. It is base on the time-domain NMR signal detected by the controller and some prior knowledge of chemical signal patterns. The desired signal can be separated from a composite signal by using an adaptive line enhancer (ALE) filter. This technique would be useful for upgrading process procedures in on-line manufacturing.

  5. Making the most of on-line recruiting.

    PubMed

    Cappelli, P

    2001-03-01

    Ninety percent of large U.S. companies are already recruiting via the Internet. By simply logging on to the Web, company recruiters can locate vast numbers of qualified candidates for jobs at every level, screen them in minutes, and contact the most promising ones immediately. The payoffs can be enormous: it costs substantially less to hire someone on-line, and the time saved is equally great. In this article, Peter Cappelli examines some of the emerging service providers and technologies--matchmakers, job boards, hiring management systems software, and applicant-screening mechanisms that test skills and record interests. He also looks at some of the strategies companies are adopting as they enter on-line labor markets. Recruiting needs to be refashioned to resemble marketing, he stresses. Accordingly, smart companies are designing Web pages, and even product ads, with potential recruits in mind. They're giving line managers authority to hire so that candidates in cyberspace aren't lost. They're building internal on-line job networks to retain talent. Integrating recruiting efforts with overall marketing campaigns, especially through coordination and identification with the company's brand, is the most important thing companies can do to ensure success in on-line hiring. Along the way, Cappelli sounds two cautionary notes. First, a human touch, not electronic contact, is vital in the last steps of a successful hiring process. Second, companies must make sure that on-line testing and hiring criteria do not discriminate against women, disabled people, workers over 40, or members of minority groups. When competition for talent is fierce, companies that master the art and science of on-line recruiting will be the ones that attract and keep the best people.

  6. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

    PubMed

    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. PMID:27260436

  7. On-line access to geoscience bibliographic citations

    USGS Publications Warehouse

    Wild, Emily C.

    2012-01-01

    On-line geoscience bibliographic citations and access points to citations are exponentially increasing as commercial, non-profit, and government agencies worldwide publish materials electronically. On-line bibliographic tools capture cited works, and open access content allows for freely obtained citations and documents. For this newsletter, citations from the numerous journals and books listed in the "Recent Papers" section of the EXPLORE newsletters from 2008-2011 were used to provide freely-accessible web sites to determine the availability of bibliographic information.

  8. Optimization of polyhydroxyalkanoates fermentations with on-line capacitance measurement.

    PubMed

    Li, Lan; Wang, Ze-Jian; Chen, Xue-Jun; Chu, Ju; Zhuang, Ying-Ping; Zhang, Si-Liang

    2014-03-01

    The aim of this work was to provide an effective methodology for optimization of the polyhydroxyalkanoates (PHAs) fermentation with Ralstonia eutropha by the on-line capacitance measurement. The present study found the capacitance values could reflect variations of microbial morphology and viability. Furthermore, oxygen uptake rate, specific oxygen uptake rate and specific growth rate were measured in real-time and compared with the capacitance value. In addition, a fed-batch control strategy based on the on-line capacitance measurement was proposed to improve the PHAs production by 22%.

  9. Psychology over the Internet: On-Line Experiences.

    PubMed

    García, V; Ahumada, L; Hinkelman, J; Muñoz, R F; Quezada, J

    2004-02-01

    The "International Symposium on Psychology over the Internet: On-Line Experiences" was held in Lima, Peru, July 2003, at the 29th InterAmerican Congress of Psychology. The main topic was the advantages and disadvantages of using this technology in the applied field of psychology. The Internet has been considered a new alternative for teaching-learning processes (virtual classroom); vocational assessment; counseling and orientation (virtual psychological consultation); and intervention focused on specific health-related problems. These experiences of on-line psychological services and their conclusions are briefly described herein. PMID:15006166

  10. Preconcentration of diluted mixed-species samples following separation and collection in a micro-nanofluidic device.

    PubMed

    Chen, Yi-Ying; Chiu, Ping-Hsien; Weng, Chen-Hsun; Yang, Ruey-Jen

    2016-01-01

    A microfluidic device consisting of a nanoscale Nafion membrane and a polydimethylsiloxane microchannel is proposed for the preconcentration of diluted multi-mixed species samples then following separation and collection. When an electric field is applied across the microchip, an accumulation of the mixed-species sample occurs at the junction between the microchannel and the membrane by means of ion concentration polarization effect. A separation of the sample then takes place due to the difference in the electrophoretic mobilities of the sample components. Finally, the component of interest is guided to a collection reservoir by manipulating the external potential configuration and is trapped in place by means of a magnetically actuated valve. The preconcentration performance of the proposed device is evaluated in both straight and convergent microchannels using a fluorescein isothiocyanate labeled bovine serum albumin (FITC-BSA) sample. It is shown that a preconcentration factor of 40 times can be achieved using a straight microchannel. By contrast, the preconcentration factor increases to 50 times when using a convergent channel. The practical feasibility of the proposed device is demonstrated by performing the preconcentration, separation, and collection of a mixed FITC-BSA and Tetramethylrhodamine sample. PMID:26909125

  11. Children's On-Line Processing of Scrambling in Japanese

    ERIC Educational Resources Information Center

    Suzuki, Takaaki

    2013-01-01

    This study investigates the on-line processing of scrambled sentences in Japanese by preschool children and adults using a combination of self-paced listening and speeded picture selection tasks. The effects of a filler-gap dependency, reversibility, and case markers were examined. The results show that both children and adults had difficulty in…

  12. On-Line Services in Medicine and Beyond

    ERIC Educational Resources Information Center

    McCarn, Davis B.; Leiter, Joseph

    1973-01-01

    Discusses the development and operation of MEDLINE which was initiated by the National Library of Medicine in 1971. This is the first generally accessible, on-line, national and international information retrieval service, and allows almost instantaneous searching of over 400,000 citations from the world's biomedical serial literature. (JR)

  13. Searching CA Condensates, On-Line and Batch.

    ERIC Educational Resources Information Center

    Kaminecki, Ronald M.; And Others

    Batch mode processing is compared, using cost-effectiveness, with on-line processing for computer-aided searching of chemical abstracts. Consideration for time, need, coverage, and adaptability are found to be the criteria by which a searcher selects a method, and sometimes both methods are used. There is a tradeoff between batch mode's slower…

  14. An On-Line Budget Information Retrieval System Design.

    ERIC Educational Resources Information Center

    Smith, Jesse L.

    Described is an On-Line Budget Information Retrieval System developed at Southern University at Baton Rouge to upgrade financial management capability. The system is designed to provide top administrators, deans, department heads, grant directors and finance or accounting staff with information less than 24 hours old. It is noted that the system…

  15. On-Line Pesticide Training with Narrated Powerpoint Presentations

    ERIC Educational Resources Information Center

    Johnson, Steven B.

    2015-01-01

    UMaine Cooperative Extension is the primary educational delivery organization for pesticide recertification credits in Maine. Shrinking budgets and staff numbers are making traditional face-to-face delivery increasingly difficult to maintain. To address this issue, on-line pesticide applicator recertification training credits were developed. The…

  16. On-Line Information Retrieval as a Scientists Tool

    ERIC Educational Resources Information Center

    Barber, A. Stephanie; And Others

    1973-01-01

    The use of an on-line information retrieval system by the scientists themselves is described. MEDUSA was designed to allow physicians to interrogate the MEDLARS data base. A Brief description is given of the system and details of an experiment to test its effectiveness. (8 references) (Author)

  17. The Nearness of You: Students & Teachers Writing On-Line.

    ERIC Educational Resources Information Center

    Edgar, Christopher, Ed.; Wood, Susan Nelson, Ed.

    This book is a guide to using new computer technologies in innovative ways to teach writing, particularly imaginative writing. The book shows how on-line technology can be a positive tool in the classroom, if the focus is on the users of the technology and the technology is integrated into the curriculum. The book is divided into five sections and…

  18. On-line diagnosis of sequential systems, 2

    NASA Technical Reports Server (NTRS)

    Sundstrom, R. J.

    1974-01-01

    The theory and techniques applicable to the on-line diagnosis of sequential systems, were investigated. A complete model for the study of on-line diagnosis is developed. First an appropriate class of system models is formulated which can serve as a basis for a theoretical study of on-line diagnosis. Then notions of realization, fault, fault-tolerance and diagnosability are formalized which have meaningful interpretations in the the context of on-line diagnosis. The diagnosis of systems which are structurally decomposed and are represented as a network of smaller systems is studied. The fault set considered is the set of faults which only affect one component system is the network. A characterization of those networks which can be diagnosed using a purely combinational detector is achieved. A technique is given which can be used to realize any network by a network which is diagnosable in the above sense. Limits are found on the amount of redundancy involved in any such technique.

  19. Gain Purchasing Power the Newfangled Way--On-Line.

    ERIC Educational Resources Information Center

    Milshtein, Amy

    1999-01-01

    Examines how San Diego State University uses computers to cut purchasing costs and boost efficiency and whether their solution can work for other business-to-business needs. How the school developed the totally self-sustaining, on-line and on-time purchasing system is discussed, including solutions to start-up problems. (GR)

  20. Bucknell On-Line Circulation System; A Library Staff View.

    ERIC Educational Resources Information Center

    Rivoire, Helena

    The Bucknell On-Line Circulation System (BLOCS) was designed to meet the requirements of a circulation system of the Ellen Clarke Bertrand Library of Bucknell University. The requirements for an automated system were, in sum: (1) a system whose operations were not only reliable but simple enough for student assistants (many of whom work only 10…

  1. The On-Line Processing of Unaccusativity in Greek Agrammatism

    ERIC Educational Resources Information Center

    Peristeri, Eleni; Tsimpli, Ianthi-Maria; Tsapkini, Kyrana

    2013-01-01

    We investigated the on-line processing of unaccusative and unergative sentences in a group of eight Greek-speaking individuals diagnosed with Broca aphasia and a group of language-unimpaired subjects used as the baseline. The processing of unaccusativity refers to the reactivation of the postverbal trace by retrieving the mnemonic representation…

  2. EPA'S ON-LINE CALCULATORS AND TRAINING COURSE

    EPA Science Inventory

    EPA has developed a suite of on-line calculators called "OnSite" for assessing transport of environmental contaminants int the subsurface. The calculators are available on the Internet at http://www.epa.gov/athens/onsite, and are divided into four categories: Parameter Estimate...

  3. On-Line NDE for Advanced Reactor Designs

    NASA Astrophysics Data System (ADS)

    Nakagawa, N.; Inanc, F.; Thompson, R. B.; Junker, W. R.; Ruddy, F. H.; Beatty, J. M.; Arlia, N. G.

    2003-03-01

    This expository paper introduces the concept of on-line sensor methodologies for monitoring the integrity of components in next generation power systems, and explains general benefits of the approach, while describing early conceptual developments of suitable NDE methodologies. The paper first explains the philosophy behind this approach (i.e. the design-for-inspectability concept). Specifically, we describe where and how decades of accumulated knowledge and experience in nuclear power system maintenance are utilized in Generation IV power system designs, as the designs are being actively developed, in order to advance their safety and economy. Second, we explain that Generation IV reactor design features call for the replacement of the current outage-based maintenance by on-line inspection and monitoring. Third, the model-based approach toward design and performance optimization of on-line sensor systems, using electromagnetic, ultrasonic, and radiation detectors, will be explained. Fourth, general types of NDE inspections that are considered amenable to on-line health monitoring will be listed. Fifth, we will describe specific modeling developments to be used for radiography, EMAT UT, and EC detector design studies.

  4. A New On-Line Resource for Psycholinguistic Studies

    ERIC Educational Resources Information Center

    Szekely, Anna; Jacobsen, Thomas; D'Amico, Simona; Devescovi, Antonella; Andonoa, Elena; Herron, Daniel; Lu, Ching Ching; Pechmann, Thomas; Pleh, Csaba; Wicha, Nicole; Federmeier, Kara; Gerdjikova, Irina; Gutierrez, Gabriel; Hung, Daisy, Hsu, Jeanne; Iyer, Gowri; Kohnert, Kathryn; Mehotcheva, Teodora; Orozco-Figueroa, Araceli; Tzeng, Angela; Tzeng, Ovid; Arevalo, Analia; Vargha, Andras; Butler, Andrew C.; Buffington, Robert; Bates, Elizabeth

    2004-01-01

    Picture naming is a widely used technique in psycholinguistic studies. Here, we describe new on-line resources that our project has compiled and made available to researchers on the world wide web at http://crl.ucsd.edu/~aszekely/ipnp/. The website provides access to a wide range of picture stimuli and related norms in seven languages. Picture…

  5. Personality Interactions and Scaffolding in On-Line Discussions

    ERIC Educational Resources Information Center

    Nussbaum, E. Michael; Hartley, Kendall; Sinatra, Gale M.; Reynolds, Ralph E.; Bendixen, Lisa D.

    2004-01-01

    The potential of on-line discussions to prompt greater reflection of course material is often stymied by a tendency of students to agree with one another rather than to formulate counter-arguments. This article describes an experiment using note starters and elaborated cases to encourage counter-argumentation and examines interactions with…

  6. On-Line Synthesis and Analysis by Mass Spectrometry

    ERIC Educational Resources Information Center

    Bain, Ryan M.; Pulliam, Christopher J.; Raab, Shannon A.; Cooks, R. Graham

    2015-01-01

    In this laboratory experiment, students learn how to use ESI to accelerate chemical synthesis and to couple it with on-line mass spectrometry for structural analysis. The Hantzsch synthesis of symmetric 1,4-dihydropyridines is a classic example of a one-pot reaction in which multiple intermediates can serve to indicate the progress of the reaction…

  7. WMI2, the Student's On-Line Symbolic Calculator

    ERIC Educational Resources Information Center

    Kovacs, Zoltan

    2011-01-01

    Student activities focused on discovering mathematics play an important role in the teaching and learning process. WebMathematics Interactive (WMI2) was developed to offer a fast and user-friendly on-line web interface to enhance the quality of both theoretical and applied mathematics courses. For the teacher, in the classroom, it provides…

  8. ON-LINE TOXICITY MONITORS AND WATERSHED EARLY WARNING SYSTEMS

    EPA Science Inventory

    A Water Quality Early Warning System using On-line Toxicity Monitors (OTMs) has been deployed in the East Fork of the Little Miami River, Clermont County, OH. Living organisms have long been used to determine the toxicity of environmental samples. With advancements in electronic ...

  9. Expanding Academic Vocabulary with an Interactive On-Line Database

    ERIC Educational Resources Information Center

    Horst, Marlise; Cobb, Tom; Nicolae, Ioana

    2005-01-01

    University students used a set of existing and purpose-built on-line tools for vocabulary learning in an experimental ESL course. The resources included concordance, dictionary, cloze-builder, hypertext, and a database with interactive self-quizzing feature (all freely available at www.lextutor.ca). The vocabulary targeted for learning consisted…

  10. On-Line Learning and the Implications for School Design

    ERIC Educational Resources Information Center

    Stack, Greg

    2011-01-01

    "Disrupting Class," published in 2008, is the story of how disruptive innovation, innovation that changes the business model organizations, will fundamentally change the American school system. The book's most startling prediction is that half of all high school classes will be on-line by 2019. In considering these predictions, the author began to…

  11. Developing an On-Line Interactive Health Psychology Module

    ERIC Educational Resources Information Center

    Upton, Dominic; Cooper, Carol

    2006-01-01

    On-line teaching material in health psychology was developed which ensured a range of students could access appropriate material for their course and level of study. This material has been developed around the concept of smaller "content chunks" which can be combined into whole units of learning (topics), and ultimately, a module. On the basis of…

  12. The On-Line Audit Revisited: Yale University.

    ERIC Educational Resources Information Center

    Weldon, Albert R., Jr.; And Others

    1984-01-01

    Yale University's on-line examination of accounting and administrative systems is discussed. Program goals are to review financial management systems at the university to identify weaknesses in internal controls, and to fulfill all audit requirements of federal grants and contracts. After outlining the quarterly audit cycle, advantages of the…

  13. The Lesson Observation On-Line (Evidence Portfolio) Platform

    ERIC Educational Resources Information Center

    Cooper, David G.

    2015-01-01

    At a time when teacher training is being moved to school-based programmes it is important to engage in a research-informed dialogue about creating more distinctive, and cost-effective 21st century models of teacher training. Three years ago I began feasibility field testing the Lesson Observation On-line (Evidence Portfolio) Platform [LOOP]…

  14. Section BB Hatch Coating; Framing Plan on Line C Lodging ...

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

    Section B-B Hatch Coating; Framing Plan on Line C Lodging Knees at Hatch; Elevation A-A Hull Framing; Section at Hatch Frame 36, Starboard Looking Aft; Midship Section Frame 37, Port Looking Aft - Steam Schooner WAPAMA, Kaiser Shipyard No. 3 (Shoal Point), Richmond, Contra Costa County, CA

  15. IOOS Data Portals and Uniform On-line Browse Capabilities

    NASA Astrophysics Data System (ADS)

    Howard, M.; Currier, R. D.; Kobara, S.; Gayanilo, F.

    2015-12-01

    The Gulf of Mexico Coastal Ocean Observing System Regional Association (GCOOS-RA) is one of eleven Regional Associations organized under the NOAA-led U.S. Integrated Ocean Observing System (IOOS) Program Office. Each of the RAs operate standards-based regional data portals designed to aggregate near real-time and historical observed data and modeled outputs from distributed providers and to offer these and derived products in standardized ways to a diverse set of users. The RA's portals are based on the IOOS Data and Communications Plan which describes the functional elements needed for an interoperable system. One of these elements is called "Uniform On-line Browse" which is an informational service designed primarily to visualize the inventory of a portal. An on-line browse service supports the end user's need to discover what parameters are available, to learn the spatial and temporal extend of the holdings, and to examine the character of the data (e.g, variability, gappiness, etc). These pieces of information help the end user decide if the data are fit for his/her purpose and to construct valid data requests. Note that on-line browse is a distinctly different activity than data analysis because it seeks to yield knowledge about the inventory and not about what the data mean. "Uniform" on-line browse is a service that takes advantage of the standardization of the data portal's data access points. Most portals represent station locations on a map. This is a view of the data inventory but these plots are rarely generated by pulling data through the standards-based services offered to the end users but through methods only available to the portal programmers. This work will present results of Uniform On-line browse tools developed within GCOOS-RA and their applicability to other RA portals.

  16. Simultaneous Electrodialytic Preconcentration and Speciation of Chromium(III) and Chromium(VI).

    PubMed

    Ohira, Shin-Ichi; Nakamura, Koretaka; Shelor, C Phillip; Dasgupta, Purnendu K; Toda, Kei

    2015-11-17

    Large amounts of chromium (Cr) compounds are used for manufacturing of various products and various chemical processes. Some inevitably find their way into the environment. Environmental Cr is dominantly inorganic and is either in the cationic +3 oxidation state or in the anionic oxochromium +6 oxidation state. The two differ dramatically in their implications; Cr(III) is essential to human nutrition and even sold as a supplement, while Cr(VI) is a potent carcinogen. Drinking water standards for chromium may be based on total Cr or Cr(VI) only. Thus, Cr speciation analysis is very important. Despite their high sensitivity, atomic spectrometric techniques or induction coupled plasma-mass spectrometry (ICP-MS) cannot directly differentiate the oxidation states. We present here a new electrodialytic separation concept. Sample analyte ions are quantitatively transferred via appropriately ionically functionalized dialysis membranes into individual receptors that are introduced into the ICP-MS. There was no significant conversion of Cr(VI) to Cr(III) or vice versa during the very short (6 s) separation process. Effects of salinity (up to ∼20 mM NaCl) can be eliminated with proper membrane functionalization and receptor optimization. With the ICP-MS detector we used, the limits of detection for either form of Cr was 0.1 μg/L without preconcentration. Up to 10-fold preconcentration was readily possible by increasing the donor solution flow rate relative to the acceptor solution flow rates. The proposed approach permits simultaneous matrix isolation, preconcentration, and chromium speciation.

  17. Amine-functionalized mesoporous polymer as potential sorbent for nickel preconcentration from electroplating wastewater.

    PubMed

    Islam, Aminul; Zaidi, Noushi; Ahmad, Hilal; Kumar, Suneel

    2015-05-01

    In this study, mesoporous glycidyl methacrylate-divinylbenzene-based chelating resin was synthesized and grafted with diethylenetriamine through epoxy ring-opening reaction. The synthesized resin was characterized by elemental analysis, infrared spectroscopy, surface area and pore size analysis, scanning electron microscopy, energy-dispersive spectroscopy, and thermogravimetry. The resin was used for the first time as an effective sorbent for the preconcentration of nickel in electroplating wastewater samples. The analytical variables like pH, flow rate for sorption/desorption, and eluate selection were systematically investigated and optimized. The uniform and monolayer sorption behavior of resin for nickel was proved by an evident fit of the equilibrium data to a Langmuir isotherm model. Under optimized conditions, the resin was observed to show a good sorption capacity of 20.25 mg g(-1) and >96% recovery of nickel even in the presence of a large number of competitive matrix ions. Its ability to extract trace amount of nickel was exhibited by low preconcentration limit (5.9 μg L(-1)). The calibration curve was found to be linear (R(2) = 0.998) in the concentration range of 6.0-400.0 μg L(-1). Coefficient of variation of less than 5 for all the analysis indicated good reproducibility. The reliability was evaluated by the analysis of standard reference material (SRM) and recovery experiments. The applicability of the resin for the systematic preconcentration of nickel is substantiated by the analysis of electroplating wastewater and river water samples. Graphical abstract ᅟ.

  18. Preconcentration and Atomization of Arsane in a Dielectric Barrier Discharge with Detection by Atomic Absorption Spectrometry.

    PubMed

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-06-01

    Atomization of arsane in a 17 W planar quartz dielectric barrier discharge (DBD) atomizer was optimized, and its performance was compared to that of a multiple microflame quartz tube atomizer (MMQTA) for atomic absorption spectrometry (AAS). Argon, at a flow rate of 60 mL min(-1), was the best DBD discharge gas. Free As atoms were also observed in the DBD with nitrogen, hydrogen, and helium discharge gases but not in air. A dryer tube filled with NaOH beads placed downstream from the gas-liquid separator to prevent residual aerosol and moisture transport to the atomizer was found to improve the response by 25%. Analytical figures of merit were comparable, reaching an identical sensitivity of 0.48 s ng (-1) As in both atomizers and limits of detection (LOD) of 0.15 ng mL(-1) As in MMQTA and 0.16 ng mL(-1) As in DBD, respectively. Compared to MMQTA, DBD provided 1 order of magnitude better resistance to interference from other hydride-forming elements (Sb, Se, and Bi). Atomization efficiency in DBD was estimated to be 100% of that reached in the MMQTA. A simple procedure of lossless in situ preconcentration of arsane was developed. Addition of 7 mL min(-1) O2 to the Ar plasma discharge resulted in a quantitative retention of arsane in the optical arm of the DBD atomizer. Complete analyte release and atomization was reached as soon as oxygen was switched off. Preconcentration efficiency of 100% was observed, allowing a decrease of the LOD to 0.01 ng mL(-1) As employing a 300 s preconcentration period. PMID:27159266

  19. A dual-adsorbent preconcentrator for a portable indoor-VOC microsensor system.

    PubMed

    Lu, C J; Zellers, E T

    2001-07-15

    The development and testing of a miniature dual-adsorbent preconcentrator for a microsensor-based analytical system designed to determine complex volatile organic chemical (VOC) mixtures encountered in indoor working environments at low part-per-billion levels is described. Candidate adsorbents were screened for thermal-desorption bandwidth and breakthrough volume against 20 volatile organic vapors and subsets thereof as a function of several relevant variables. A glass capillary (1.1 mm i.d.) packed with 3.4 mg of Carbopack X and 1.2 mg of Carboxen 1000 provides sufficient capacity for a 1-L dry-air sample containing all 20 vapors at concentrations of 100 ppb as well as providing a composite half-height peak width of <3 s at a desorption temperature of 300 degrees C and a flow rate of 4 mL/min. Required adsorbent masses increase to 7.0 and 1.5 mg, respectively, for the same mixture at component concentrations of 1 ppm. Vapor breakthrough volumes for the Carbopack X are unaffected by humidity from 0 to 100%RH, but those for the Carboxen 1000 are significantly reduced, requiring an additional 0.9 mg of the latter to avoid premature breakthrough at the 100 ppb level. Good peak shapes, efficient chromatographic separation of preconcentrated sample mixture components, and detection limits in the low-parts-per-billion range using an integrated surface-acoustic-wave (SAW) sensor are achieved. Preconcentrator design and operating parameters are considered in terms of the vapor bed-residence times and breakthrough volumes in the context of the modified Wheeler equation.

  20. A dual-adsorbent preconcentrator for a portable indoor-VOC microsensor system.

    PubMed

    Lu, C J; Zellers, E T

    2001-07-15

    The development and testing of a miniature dual-adsorbent preconcentrator for a microsensor-based analytical system designed to determine complex volatile organic chemical (VOC) mixtures encountered in indoor working environments at low part-per-billion levels is described. Candidate adsorbents were screened for thermal-desorption bandwidth and breakthrough volume against 20 volatile organic vapors and subsets thereof as a function of several relevant variables. A glass capillary (1.1 mm i.d.) packed with 3.4 mg of Carbopack X and 1.2 mg of Carboxen 1000 provides sufficient capacity for a 1-L dry-air sample containing all 20 vapors at concentrations of 100 ppb as well as providing a composite half-height peak width of <3 s at a desorption temperature of 300 degrees C and a flow rate of 4 mL/min. Required adsorbent masses increase to 7.0 and 1.5 mg, respectively, for the same mixture at component concentrations of 1 ppm. Vapor breakthrough volumes for the Carbopack X are unaffected by humidity from 0 to 100%RH, but those for the Carboxen 1000 are significantly reduced, requiring an additional 0.9 mg of the latter to avoid premature breakthrough at the 100 ppb level. Good peak shapes, efficient chromatographic separation of preconcentrated sample mixture components, and detection limits in the low-parts-per-billion range using an integrated surface-acoustic-wave (SAW) sensor are achieved. Preconcentrator design and operating parameters are considered in terms of the vapor bed-residence times and breakthrough volumes in the context of the modified Wheeler equation. PMID:11476247

  1. Exploration geochemical technique for the determination of preconcentrated organometallic halides by ICP-AES

    USGS Publications Warehouse

    Motooka, J.M.

    1988-01-01

    An atomic absorption extraction technique which is widely used in geochemical exploration for the determination of Ag, As, Au, Bi, Cd, Cu, Mo, Pb, Sb, and Zn has been modified and adapted to a simultaneous inductively coupled plasma-atomic emission instrument. the experimental and operating parameters are described for the preconcentration of the metals into their organometallic halides and for the determination of the metals. Lower limits of determination are equal to or improved over those for flame atomic absorption (except Au) and ICP results are very similar to the accepted AA values, with precision for the ICP data in excess of that necessary for exploration purposes.

  2. Preconcentration of heavy metals in urine and quantification by inductively coupled plasma atomic emission spectrometry.

    PubMed

    López-Artíguez, M; Cameán, A; Repetto, M

    1993-01-01

    This paper describes a method for the determination of heavy metals (Co, Ni, Cu, Cd, Pb) in urine by inductively coupled plasma atomic emission spectrometry (ICP-AES). The method proposed requires purification of the samples with activated charcoal under acidic conditions before preconcentration by complexation with ammonium pyrrolidinedithiocarbamate (APDC). The formed complexes are extracted with methyl isobutyl ketone (MIBK) and the resulting residue is finally digested under acid oxidant conditions. Because of its low detection limit (below 10 micrograms/L), this procedure can be applied conveniently for toxicological diagnostic purposes. PMID:8429621

  3. Automatic Delineation of On-Line Head-And-Neck Computed Tomography Images: Toward On-Line Adaptive Radiotherapy

    SciTech Connect

    Zhang Tiezhi . E-mail: tiezhi.zhang@beaumont.edu; Chi Yuwei; Meldolesi, Elisa; Yan Di

    2007-06-01

    Purpose: To develop and validate a fully automatic region-of-interest (ROI) delineation method for on-line adaptive radiotherapy. Methods and Materials: On-line adaptive radiotherapy requires a robust and automatic image segmentation method to delineate ROIs in on-line volumetric images. We have implemented an atlas-based image segmentation method to automatically delineate ROIs of head-and-neck helical computed tomography images. A total of 32 daily computed tomography images from 7 head-and-neck patients were delineated using this automatic image segmentation method. Manually drawn contours on the daily images were used as references in the evaluation of automatically delineated ROIs. Two methods were used in quantitative validation: (1) the dice similarity coefficient index, which indicates the overlapping ratio between the manually and automatically delineated ROIs; and (2) the distance transformation, which yields the distances between the manually and automatically delineated ROI surfaces. Results: Automatic segmentation showed agreement with manual contouring. For most ROIs, the dice similarity coefficient indexes were approximately 0.8. Similarly, the distance transformation evaluation results showed that the distances between the manually and automatically delineated ROI surfaces were mostly within 3 mm. The distances between two surfaces had a mean of 1 mm and standard deviation of <2 mm in most ROIs. Conclusion: With atlas-based image segmentation, it is feasible to automatically delineate ROIs on the head-and-neck helical computed tomography images in on-line adaptive treatments.

  4. On-line sequential injection dispersive liquid-liquid microextraction system for flame atomic absorption spectrometric determination of copper and lead in water samples.

    PubMed

    Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

    2009-06-30

    A simple, sensitive and powerful on-line sequential injection (SI) dispersive liquid-liquid microextraction (DLLME) system was developed as an alternative approach for on-line metal preconcentration and separation, using extraction solvent at microlitre volume. The potentials of this novel schema, coupled to flame atomic absorption spectrometry (FAAS), were demonstrated for trace copper and lead determination in water samples. The stream of methanol (disperser solvent) containing 2.0% (v/v) xylene (extraction solvent) and 0.3% (m/v) ammonium diethyldithiophosphate (chelating agent) was merged on-line with the stream of sample (aqueous phase), resulting a cloudy mixture, which was consisted of fine droplets of the extraction solvent dispersed entirely into the aqueous phase. By this continuous process, metal chelating complexes were formed and extracted into the fine droplets of the extraction solvent. The hydrophobic droplets of organic phase were retained into a microcolumn packed with PTFE-turnings. A portion of 300 microL isobutylmethylketone was used for quantitative elution of the analytes, which transported directly to the nebulizer of FAAS. All the critical parameters of the system such as type of extraction solvent, flow-rate of disperser and sample, extraction time as well as the chemical parameters were studied. Under the optimum conditions the enhancement factor for copper and lead was 560 and 265, respectively. For copper, the detection limit and the precision (R.S.D.) were 0.04 microg L(-1) and 2.1% at 2.0 microg L(-1) Cu(II), respectively, while for lead were 0.54 microg L(-1) and 1.9% at 30.0 microg L(-1) Pb(II), respectively. The developed method was evaluated by analyzing certified reference material and applied successfully to the analysis of environmental water samples. PMID:19376348

  5. On-line object feature extraction for multispectral scene representation

    NASA Technical Reports Server (NTRS)

    Ghassemian, Hassan; Landgrebe, David

    1988-01-01

    A new on-line unsupervised object-feature extraction method is presented that reduces the complexity and costs associated with the analysis of the multispectral image data and data transmission, storage, archival and distribution. The ambiguity in the object detection process can be reduced if the spatial dependencies, which exist among the adjacent pixels, are intelligently incorporated into the decision making process. The unity relation was defined that must exist among the pixels of an object. Automatic Multispectral Image Compaction Algorithm (AMICA) uses the within object pixel-feature gradient vector as a valuable contextual information to construct the object's features, which preserve the class separability information within the data. For on-line object extraction the path-hypothesis and the basic mathematical tools for its realization are introduced in terms of a specific similarity measure and adjacency relation. AMICA is applied to several sets of real image data, and the performance and reliability of features is evaluated.

  6. PHENIX on-line and off-line computing

    NASA Astrophysics Data System (ADS)

    Adler, S. S.; Chujo, T.; Desmond, E. J.; Ewell, L.; Ghosh, T. K.; Haggerty, J. S.; Ichihara, T.; Jacak, B. V.; Johnson, S. C.; Kehayias, H.-J.; Lauret, J.; Maguire, C. F.; Messer, M.; Mioduszewski, S.; Mitchell, J. T.; Morrison, D. P.; Ojha, I. D.; Pinkenburg, C. H.; Pollack, M.; Pope, K.; Purschke, M. L.; Sorensen, S.; Sourikova, I.; Thomas, T. L.; Velkovsky, M.; Watanabe, Y.; Witzig, C.; Yokkaichi, S.; Zajc, W. A.; PHEN. I. X. Collaboration

    2003-03-01

    Data handling in PHENIX is carried out by the On-Line Computing System (ONCS) and Off-Line Computing System (Off-Line). ONCS provides the overall control and monitoring of the front-end electronics, trigger and data acquisition system and detector ancillary systems. It configures and initializes the on-line system, monitors and controls the data flow, coordinates calibration processes, interlocks the data acquisition process with the slow control subsystems and performs a number of other functions. ONCS uses CORBA software to monitor and control the hardware. Off-Line provides all aspects of data handling not directly connected to the collection of data and monitoring, such as event simulation and reconstruction, data analysis and information management. The impact of the unprecedented data volumes on the design is presented, along with a detailed discussion of the tasks and methods of simulating, obtaining and monitoring the data.

  7. On-line analyzers to distributed control system linking

    SciTech Connect

    Peterson, S.F.; Buchanan, B.R.; Sanders, M.A.

    1990-01-01

    The Analytical Development Section (ADS) of the Savannah River Laboratory is developing on-line analyzers to monitor various site processes. Data from some of the on-line analyzers (OLA's) will be used for process control by distributed control systems (DCS's) such as the Fisher PRoVOX. A problem in the past has been an efficient and cost effective way to get analyzer data onto the DCS data highway. ADS is developing a system to accomplish the linking of OLA's to PRoVOX DCS's. The system will be described, and results of operation in a research and development environment given. Plans for the installation in the production environment will be discussed.

  8. On-Line Monitoring of Plan Execution: a Distributed Approach

    NASA Astrophysics Data System (ADS)

    Micalizio, Roberto; Torasso, Pietro

    The paper introduces and formalizes a distributed approach for the model-based monitoring of the execution of a plan, where concurrent actions are carried on by a team of mobile robots in a partially observable environment. Each robot is monitored on-line by an agent that has the task of tracking all the possible evolutions both under nominal and faulty behavior of the robot and to estimate the belief state at each timeinstant. The strategy for deriving local solutions which are globally consistent is formalized. The distributed monitoring provides on-line feedback to a system supervisor which has to decide whether building a new plan as consequence of actions failure. The feasibility of the approach and the gain in the performance are shown by comparing experimental results of the proposed approach with a centralized one.

  9. On-line monitoring: Improving hydro maintenance and operations

    SciTech Connect

    Byers, W.

    1996-02-01

    Expert monitoring systems provide plant owners and operators with a means of judging the condition of hydropower equipment before problems arise. The systems also produce information that can be used to maximize efficiency and output and minimize costs. This article is a discussion of such on-line systems. Technical advances providing the basis for these systems and general applications of these systems are reviewed. Specific applications at the Hausling pumped storage project and the Itaipu hydroelectric project are discussed.

  10. On-line fluorometric microbiological analysis for life support systems

    NASA Astrophysics Data System (ADS)

    Schlager, Kenneth J.

    1992-07-01

    Fluorometric data, both spectral and time-resolved, are characterized by background luminescence and interfering, overlapping spectra from various living and nonliving fluorometric sources. Sophisticated pattern recognition techniques are used to identify and quantify microbial species of interest in the complex measurement environment. It is concluded that advanced pattern recognition methods based on neural networks supervised by genetic algorithms have been quite successful in identifying and quantifying bacteria and fungi in continuous on-line monitoring applications.

  11. Development and Evaluation of Nanoemulsifying Preconcentrate of Curcumin for Colon Delivery

    PubMed Central

    Wadhwa, Jyoti; Asthana, Abhay; Shilakari, Gyati; Chopra, Arun Kumar; Singh, Ranjit

    2015-01-01

    The present study aimed to develop and optimize a nanoemulsifying preconcentrate formulation of curcumin with good emulsification ability and optimal globule size, for controlled targeting in colon. Content of formulation variables, namely, X1 (Peceol), X2 (Cremophor-EL), and X3 (Transcutol HP), were optimized by Box-Behnken design of experiments for its impact on mean globule size (Y1), emulsification time (Y2), and time required for drug release (85%) in phosphate buffer (pH 7.2), t85% (Y3). Transmission electron micrographs confirmed that there is no coalescence among globules, with size range concordant with the globule size analysis by dynamic light scattering technique (100 nm). 3D plots indicated that concentration of formulation ingredients significantly influences the formulation properties (globule size, emulsification time, and drug release). In vitro release profile (in phosphate buffer; pH 7.2) represents the fact that more than 50% of the drug was released within initial 15 min whereas in vivo release showed limited systemic absorption (Cmax 200 ng/mL) of curcumin. Stability study ensures the protection of drug in alkaline media which may further confirm the localised delivery of drug to colonic region. Study demonstrated that the nanoemulsifying preconcentrate can be a promising system for the colon specific delivery of curcumin to treat local pathologies. PMID:25861680

  12. Vapor generation - atomic spectrometric techniques. Expanding frontiers through specific-species preconcentration. A review.

    PubMed

    Gil, Raúl A; Pacheco, Pablo H; Cerutti, Soledad; Martinez, Luis D

    2015-05-22

    We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid-liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field.

  13. Double preconcentration of trace amounts of cadmium in nail samples and measurement by differential pulse voltammetry.

    PubMed

    Shahi, Somayeh; Nateghi, Mohammad Reza

    2015-04-01

    Cadion was coated on carbon powder and used as a solid phase for selective extraction and preconcentration of cadmium ions. Complexed cadmium ions were eluted from solid phase by 5 mL, nitric acid (2.0 M) with the flow rate of 2 mL min(-1).The resulted solution was used for accumulation of the cadmium metal at the surface of the carbon paste electrode at -1.3 V reduction potential. Finally, cadmium was reoxidized and the differential pulse voltammogram recorded at the potential range of -0.55 to -0.2 V. Calibration graph was plotted in the concentration range of 0.5-50 μg L(-1) of cadmium. Detection limit 0.06 μg L(-1) was calculated based on the 3 Sb/m. The RSD was 9.13 % (n = 4) for cadmium concentration of 10 μg L(-1) with preconcentration factor of 100. Method was successfully used for the determination of cadmium in finger nail samples and after spiking the samples, the recoveries were evaluated >96 %.

  14. Multi-parameter on-line coal bulk analysis

    SciTech Connect

    1999-02-01

    This was a four-year grant that was given a no cost extension for one more year. The purpose of the grant was to develop a pulsed neutron-based technique that could measure on-line all the major and minor elements in coal. Such measurements would allow the continuous monitoring of bulk parameters such as coal heating value (BTU/lb), volatile matter, moisture etc., deemed important to the coal industry. Such parameters, along with the continuous measurement of elements such as sulfur and sodium, are of major economic and environmental concern, and their measurement would assist in a more efficient use of the coal-fired boilers, as well as limiting emissions controlled by the 1990 Clean Air Act Amendments. It was hoped that this study would lead to the development of a technique able to create a marketable product, an On-Line Elemental Coal Analyzer. The study was separated in the following major parts: (1) Devise an efficient system for the detection of gamma rays; (2) Prior to experimentation, perform modeling and simulations for items such as detector shielding, coal sample configuration, and neutron tube collimation; (3) Develop a computer code for data reduction and analysis; (4) Measure the elemental composition of various coal samples; and (5) Design a prototype, on-line elemental coal analyzer, based on the PFTNA principle.

  15. The new on-line Czech Food Composition Database.

    PubMed

    Machackova, Marie; Holasova, Marie; Maskova, Eva

    2013-10-01

    The new on-line Czech Food Composition Database (FCDB) was launched on http://www.czfcdb.cz in December 2010 as a main freely available channel for dissemination of Czech food composition data. The application is based on a complied FCDB documented according to the EuroFIR standardised procedure for full value documentation and indexing of foods by the LanguaL™ Thesaurus. A content management system was implemented for administration of the website and performing data export (comma-separated values or EuroFIR XML transport package formats) by a compiler. Reference/s are provided for each published value with linking to available freely accessible on-line sources of data (e.g. full texts, EuroFIR Document Repository, on-line national FCDBs). LanguaL™ codes are displayed within each food record as searchable keywords of the database. A photo (or a photo gallery) is used as a visual descriptor of a food item. The application is searchable on foods, components, food groups, alphabet and a multi-field advanced search.

  16. On-Line Fringe Tracking and Prediction at IOTA

    NASA Technical Reports Server (NTRS)

    Wilson, Edward; Mah, Robert; Lau, Sonie (Technical Monitor)

    1999-01-01

    The Infrared/Optical Telescope Array (IOTA) is a multi-aperture Michelson interferometer located on Mt. Hopkins near Tucson, Arizona. To enable viewing of fainter targets, an on-line fringe tracking system is presently under development at NASA Ames Research Center. The system has been developed off-line using actual data from IOTA, and is presently undergoing on-line implementation at IOTA. The system has two parts: (1) a fringe tracking system that identifies the center of a fringe packet by fitting a parametric model to the data; and (2) a fringe packet motion prediction system that uses characteristics of past fringe packets to predict fringe packet motion. Combined, this information will be used to optimize on-line the scanning trajectory, resulting in improved visibility of faint targets. Fringe packet identification is highly accurate and robust (99% of the 4000 fringe packets were identified correctly, the remaining 1% were either out of the scan range or too noisy to be seen) and is performed in 30-90 milliseconds on a Pentium II-based computer. Fringe packet prediction, currently performed using an adaptive linear predictor, delivers a 10% improvement over the baseline of predicting no motion.

  17. Designing effective on-line continuing medical education.

    PubMed

    Zimitat, Craig

    2001-03-01

    The Internet, and new information and communication technologies available through the Internet, provides medical educators with an opportunity to develop unique on-line learning environments with real potential to improve physicians' knowledge and effect change in their clinical practice. There are approximately 100 websites offering on-line CME courses in the USA alone. However, few of these CME courses appear to be based on sound educational principles or CME research and may have little chance of achieving the broader goals of CME. The majority of these courses closely resemble their traditional counterparts (e.g. paper-based books are now electronic books) and appear to be mere substitutions for old-technology CME resources. Whilst some CME providers add unique features of the Internet to enrich their websites, they do not employ strategies to optimize the learning opportunities afforded by this new technology. The adoption of adult learning principles, reflective practice and problem-based approaches can be used as a foundation for sound CME course design. In addition, knowledge of Internet technology and the learning opportunities it affords, together with strategies to maintain participation and new assessment paradigms, are all needed for developing online CME. We argue for an evidence-based and strategic approach to the development of on-line CME courses designed to enhance physician learning and facilitate change in clinical behaviour.

  18. Review of trigger and on-line processors at SLAC

    SciTech Connect

    Lankford, A.J.

    1984-07-01

    The role of trigger and on-line processors in reducing data rates to manageable proportions in e/sup +/e/sup -/ physics experiments is defined not by high physics or background rates, but by the large event sizes of the general-purpose detectors employed. The rate of e/sup +/e/sup -/ annihilation is low, and backgrounds are not high; yet the number of physics processes which can be studied is vast and varied. This paper begins by briefly describing the role of trigger processors in the e/sup +/e/sup -/ context. The usual flow of the trigger decision process is illustrated with selected examples of SLAC trigger processing. The features are mentioned of triggering at the SLC and the trigger processing plans of the two SLC detectors: The Mark II and the SLD. The most common on-line processors at SLAC, the BADC, the SLAC Scanner Processor, the SLAC FASTBUS Controller, and the VAX CAMAC Channel, are discussed. Uses of the 168/E, 3081/E, and FASTBUS VAX processors are mentioned. The manner in which these processors are interfaced and the function they serve on line is described. Finally, the accelerator control system for the SLC is outlined. This paper is a survey in nature, and hence, relies heavily upon references to previous publications for detailed description of work mentioned here. 27 references, 9 figures, 1 table.

  19. Problem formulation, metrics, open government, and on-line collaboration

    NASA Astrophysics Data System (ADS)

    Ziegler, C. R.; Schofield, K.; Young, S.; Shaw, D.

    2010-12-01

    Problem formulation leading to effective environmental management, including synthesis and application of science by government agencies, may benefit from collaborative on-line environments. This is illustrated by two interconnected projects: 1) literature-based evidence tools that support causal assessment and problem formulation, and 2) development of output, outcome, and sustainability metrics for tracking environmental conditions. Specifically, peer-production mechanisms allow for global contribution to science-based causal evidence databases, and subsequent crowd-sourced development of causal networks supported by that evidence. In turn, science-based causal networks may inform problem formulation and selection of metrics or indicators to track environmental condition (or problem status). Selecting and developing metrics in a collaborative on-line environment may improve stakeholder buy-in, the explicit relevance of metrics to planning, and the ability to approach problem apportionment or accountability, and to define success or sustainability. Challenges include contribution governance, data-sharing incentives, linking on-line interfaces to data service providers, and the intersection of environmental science and social science. Degree of framework access and confidentiality may vary by group and/or individual, but may ultimately be geared at demonstrating connections between science and decision making and supporting a culture of open government, by fostering transparency, public engagement, and collaboration.

  20. DEVELOPMENT OF AN ON-LINE COAL WASHABILITY ANALYZER

    SciTech Connect

    J.D. Miller; C.L. Lin; G.H. Luttrell; G.T. Adel; Barbara Marin

    2001-06-26

    Washability analysis is the basis for nearly all coal preparation plant separations. Unfortunately, there are no on- line techniques for determining this most fundamental of all coal cleaning information. In light of recent successes at the University of Utah, it now appears possible to determine coal washability on-line through the use of x-ray computed tomography (CT) analysis. The successful development of such a device is critical to the establishment of process control and automated coal blending systems. In this regard, Virginia Tech, Terra Tek Inc., and U.S. coal producers have joined with the University of Utah and to undertake the development of an X-ray CT-based on- line coal washability analyzer with financial assistance from DOE. Each project participant brought special expertise to the project in order to create a new dimension in coal cleaning technology. The project involves development of appropriate software and extensive testing/evaluation of well-characterized coal samples from operating coal preparation plants. Data collected to date suggest that this new technology is capable of serving as a universal analyzer that can not only provide washability analysis, but also particle size distribution analysis, ash analysis, and perhaps pyritic sulfur analysis.

  1. Development of an On-Line Coal Washability Analyzer

    SciTech Connect

    C. L. Lin; G. H. Luttrell; G. T. Adel; Jan D. Miller

    1998-03-31

    Washability analysis is the basis for nearly all coal preparation plant separations. Unfortunately, there are no on-line techniques for determining this most fundamental of all coal cleaning information. In light of recent successes at the University of Utah, it now appears possible to determine coal washability on-line through the use of x-ray computed tomography (CT) analysis. The successful development of such a device is critical to the establishment of process control and automated coal blending systems. In this regard, Virginia Tech, Terra Tek Inc., and Cyprus-Amax Coal Company have joined with the University of Utah and agreed to undertake the development of a x-ray CT-based on-line coal washability analyzer with financial assistance from DOE. The three-year project will cost $594,571, of which 33% ($194,575) will be cost-shared by the participants. The project will involve development of appropriate software and extensive testing/evaluation of well-characterized coal samples from three coal preparation plants. Each project participant brings special expertise to the project which is expected to create a new dimension in coal cleaning technology. Finally, it should be noted that the analyzer may prove to be a universal analyzer capable of providing not only washability analysis, but also particle size distribution analysis, ash analysis and perhaps pyritic sulfur analysis.

  2. Preconcentration and Separation of Mixed-Species Samples Near a Nano-Junction in a Convergent Microchannel.

    PubMed

    Chiu, Ping-Hsien; Weng, Chen-Hsun; Yang, Ruey-Jen

    2015-01-01

    A fluidic microchip incorporating a convergent microchannel and a Nafion-nanoporous membrane is proposed for the preconcentration and separation of multi-species samples on a single platform. In the device, sample preconcentration is achieved by means of the ion concentration polarization effect induced at the micro/nano interface under the application of an external electric field, while species separation is achieved by exploiting the different electrophoretic mobilities of the sample components. The experimental results show that the device is capable of detecting C-reactive protein (CRP) with an initial concentration as low as 9.50 × 10(-6) mg/L given a sufficient preconcentration time and driving voltage. In addition, it is shown that a mixed-species sample consisting of three negatively-charged components (bovine serum albumin (BSA), tetramethylrhodamine(TAMRA) isothiocyanate-Dextran and fluorescent polymer beads) can be separated and preconcentrated within 20 min given a driving voltage of 100 V across 1 cm microchannel in length. In general, the present results confirm the feasibility of the device for the immunoassay or detection of various multi-species samples under low concentration in the biochemical and biomedical fields. The novel device can therefore improve the detection limit of traditional medical facilities. PMID:26690167

  3. Salting-out solvent extraction for the off-line preconcentration of benzalkonium chloride in capillary electrophoresis.

    PubMed

    So, T S; Huie, C W

    2001-07-01

    The use of salting-out effect for the off-line preconcentration of charged analytes in capillary electrophoresis is demonstrated for the first time. Using benzalkonium chloride (BAK) as model compound, a mixture of cationic surfactants consisting of even-numbered alkylbenzyl quaternary ammonium homologues (C8-C18), the addition of appropriate amounts of sodium chloride and acetonitrile in the sample solution (2 mL sample volume) was found to be capable of providing ca. 40-fold enhancement in detection sensitivity. In addition to affording a preconcentrating effect due to the extraction of BAK in the smaller volume water-miscible organic solvent phase (acetonitrile), the organic solvent also serves to improve the peak area and shape of the longer chain surfactants. Optimal experimental conditions, such as volume of acetonitrile and concentration of sodium chloride, for the preconcentration of BAK with good preconcentration factors and reproducibility were investigated. The usefulness of the present method was demonstrated for the improved determination of BAK present in commercially available industrial and pharmaceutical products.

  4. Separation and preconcentration of trace amounts of aluminum ions in surface water samples using different analytical techniques.

    PubMed

    Khan, Sumaira; Kazi, Tasneem G; Baig, Jameel A; Kolachi, Nida F; Afridi, Hassan I; Shah, Abdul Q; Kandhro, Ghulam A; Kumar, Sham

    2009-11-15

    A separation/preconcentration of aluminum (III) (Al(3+)) has been developed to overcome the problem of high matrix species, which may interfere with the determination of trace quantity of Al(3+) in natural water samples. The separation of Al(3+) in water samples was carried out from interfering cations by complexing them with 2-methyle 8-hyroxyquinoline (quinaldine) on activated silica. Whereas the separated trace amounts of Al(3+) was preconcentrated by cloud point extraction (CPE), as prior step to its determination by spectrofluorimetry (SPF) and flame atomic absorption spectrometry (FAAS). The Al(3+) react with 8-hydroxyquinoline (oxine) and then entrapped in non-ionic surfactant Triton X-114. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of oxine and Triton X-114, equilibration temperature and time period for shaking were investigated in detail. The validity of separation/preconcentration of Al(3+) was checked by certified reference material of water (SRM-1643e). After optimization of the complexation and extraction conditions, a preconcentration factor of 20 was obtained for Al(3+) in 10 mL of natural water samples. The relative standard deviation for 6 replicates containing 100 microg L(-1) of Al(3+) was 5.41 and 4.53% for SPF and FAAS, respectively. The proposed method has been applied for determination of trace amount of Al(3+) in natural water samples with satisfactory results. PMID:19782206

  5. Concentration-enhanced rapid detection of human chorionic gonadotropin (hCG) on a Au surface using a nanofluidic preconcentrator

    PubMed Central

    Lee, Jeong Hoon; Han, Jongyoon

    2010-01-01

    Here, we report a new method of concentration-enhanced binding kinetics for a rapid immunoassay screening test on a gold surface in a poly(dimethylsiloxane) (PDMS) microfluidic chip format. The use of alkylthiolate self-assembled monolayers on gold surfaces of a PDMS-glass microchip resulted in accelerated binding kinetics of Human chorionic gonadotropin (hCG) at an electrokinetic trapping zone. We used a PBS solution (buffer concentration ~ 150 mM), not a dibasic buffer system (~10 mM), for the dynamic preconcentrating operation and the preconcentration of cy3 labeled streptavidin onto biotinylated Au surface revealed that the binding kinetics of the protein were linearly proportional to the concentration profile of the preconcentration plug. We showed rapid detection of hCG in the clinical range with a shorten assay time of 10 min. Also, we demonstrated that the amount of sample needed were detection was decreased from ~4 mL to ~25 μL in the standard serum tests. The enhanced binding kinetics between hcG Ag-Ab via preconcentration showed good feasibility for use in a rapid immunoassay screening test. PMID:20953263

  6. Preconcentration and Separation of Mixed-Species Samples Near a Nano-Junction in a Convergent Microchannel

    PubMed Central

    Chiu, Ping-Hsien; Weng, Chen-Hsun; Yang, Ruey-Jen

    2015-01-01

    A fluidic microchip incorporating a convergent microchannel and a Nafion-nanoporous membrane is proposed for the preconcentration and separation of multi-species samples on a single platform. In the device, sample preconcentration is achieved by means of the ion concentration polarization effect induced at the micro/nano interface under the application of an external electric field, while species separation is achieved by exploiting the different electrophoretic mobilities of the sample components. The experimental results show that the device is capable of detecting C-reactive protein (CRP) with an initial concentration as low as 9.50 × 10−6 mg/L given a sufficient preconcentration time and driving voltage. In addition, it is shown that a mixed-species sample consisting of three negatively-charged components (bovine serum albumin (BSA), tetramethylrhodamine(TAMRA) isothiocyanate-Dextran and fluorescent polymer beads) can be separated and preconcentrated within 20 min given a driving voltage of 100 V across 1 cm microchannel in length. In general, the present results confirm the feasibility of the device for the immunoassay or detection of various multi-species samples under low concentration in the biochemical and biomedical fields. The novel device can therefore improve the detection limit of traditional medical facilities. PMID:26690167

  7. Toward the use of surface modified activated carbon in speciation: selective preconcentration of selenite and selenate in environmental waters.

    PubMed

    Tsoi, Yeuk-Ki; Leung, Kelvin Sze-Yin

    2011-04-22

    This paper describes a novel application of tetrabutylammonium hydroxide-modified activated carbon (AC-TBAH) to the speciation of ultra-trace Se(IV) and Se(VI) using LC-ICP-DRC-MS. The anion exchange functionality was immobilized onto the AC surface enables selective preconcentration of inorganic Se anions in a wide range of working pHs. Simultaneous retention and elution of both analytes, followed by subsequent analysis with LC-ICP-DRC-MS, allows to accomplish speciation analysis in natural samples without complicated redox pre-treatment. The laboratory-made column of immobilized AC (0.4 g of sorbent packed in a 6 mL syringe barrel) has achieved analyte enrichment factors of 76 and 93, respectively, for Se(IV) and Se(VI), thus proving its superior preconcentration efficiency and selectivity over common AC. The considerable enhancement in sensitivity achieved by using the preconcentration column has improved the method's detection limits to 1.9-2.2 ng L(-1), which is a 100-fold improvement compared with direct injection. The analyte recoveries from heavily polluted river matrix were between 95.3 and 107.7% with less than 5.0% RSD. The robustness of the preconcentration and speciation method was validated by analysis of natural waters collected from rivers and reservoirs in Hong Kong. The modified AC material is hence presented as a low-cost yet robust substitute for conventional anion exchange resins for routine applications.

  8. SELECTIVE TRACE ENRICHMENT BY IMMUNOAFFINITY CAPILLARY ELECTROCHROMATOGRAPHY ON-LINE WITH CAPILLARY ZONE ELECTROPHORESIS - LASER-INDUCED FLUORESCENCE

    EPA Science Inventory

    Limited by the lack of a sensitive, universal detector, many capillary-based liquid-phase separation techniques might benefit from techniques that overcome modest concentration sensitivity by preconcentrating large injection volumes. The work presented employs selective solid-ph...

  9. A Refreshable, On-line Cache for HST Data Retrieval

    NASA Astrophysics Data System (ADS)

    Fraquelli, Dorothy A.; Ellis, Tracy A.; Ridgaway, Michael; DPAS Team

    2016-01-01

    We discuss upgrades to the HST Data Processing System, with an emphasis on the changes Hubble Space Telescope (HST) Archive users will experience. In particular, data are now held on-line (in a cache) removing the need to reprocess the data every time they are requested from the Archive. OTFR (on the fly reprocessing) has been replaced by a reprocessing system, which runs in the background. Data in the cache are automatically placed in the reprocessing queue when updated calibration reference files are received or when an improved calibration algorithm is installed. Data in the on-line cache are expected to be the most up to date version. These changes were phased in throughout 2015 for all active instruments.The on-line cache was populated instrument by instrument over the course of 2015. As data were placed in the cache, the flag that triggers OTFR was reset so that OTFR no longer runs on these data. "Hybrid" requests to the Archive are handled transparently, with data not yet in the cache provided via OTFR and the remaining data provided from the cache. Users do not need to make separate requests.Users of the MAST Portal will be able to download data from the cache immediately. For data not in the cache, the Portal will send the user to the standard "Retrieval Options Page," allowing the user to direct the Archive to process and deliver the data.The classic MAST Search and Retrieval interface has the same look and feel as previously. Minor changes, unrelated to the cache, have been made to the format of the Retrieval Options Page.

  10. On-line estimation of biodegradation in an unsaturated soil.

    PubMed

    Schoefs, O; Perrier, M; Dochain, D; Samson, R

    2003-11-01

    The objective of this study was to develop a model-based estimator of biodegradation in unsaturated soil. This would allow real-time assessment of the efficiency of treatment bioprocesses, such as bioventilation and biopile, and eventually permit optimization through the implementation of control strategies. Based on a reduced-order model, an asymptotic observer was designed to estimate on-line the contaminant concentration, using carbon dioxide measurement. Two observer-based estimators were built to approximate: (1) the specific microbial growth rate; and (2) the biocontact kinetics representing the soil resistance to contaminant biodegradation. State observers and parameter estimators were confronted with the experimental results of biodegradation in microcosms. Hexadecane was used as the model compound, representing petroleum hydrocarbons. Three water contents, corresponding to 20%, 50% and 80% of the water-holding capacity, were tested. The asymptotic observer is able to predict hexadecane depletion with an error on the overall time trajectories of 13%, 8% and 4% for the dry, intermediate and wet soils, respectively, which is acceptable given that all the biokinetic parameters were identified from a biodegradation experiment in liquid phase. The observer-based estimator of the specific microbial growth rate, based on the CO(2) measurement, was successfully calibrated using the off-line measurements of hexadecane as validation data, and allowed estimation of the time when biodegradation switched from a microbial to a biocontact limitation. The biocontact kinetics was also identified on-line, using an estimator based on the hexadecane not in biocontact. These results are very encouraging with respect to the potential for on-line assessment of the performance of treatment bioprocesses in unsaturated soils.

  11. Anisotropic. cap alpha. -emission of on-line separated isotopes

    SciTech Connect

    Wouters, J.; Vandeplassche, D.; van Walle, E.; Severijns, N.; Van Haverbeke, J.; Vanneste, L.

    1987-12-10

    The technical realization of particle detection at very low temperatures (4K) has made it possible to study for the first time the anisotropic ..cap alpha..-decay of oriented nuclei which have been produced, separated and implanted on line. The measured ..cap alpha..-angular distributions reveal surprising new results on nuclear aspects as well as in solid state physics. The nuclear structure information from these data questions the older ..cap alpha..-decay theoretical interpretation and urges for a reaxamination of the earliest work on anisotropic ..cap alpha..-decay.

  12. On-line composition with laser-based techniques

    SciTech Connect

    Finch, F.T.; Hartford, A. Jr.

    1982-01-01

    Current methods for determining the composition of coal gasification streams generally involve sampling, some treatment, and inherent delay times prior to analysis. Optical instrumentation, on the other hand, provides the potential for on-line, rapid-response monitoring of gasifier streams. Among the optical technques that appear quite promising for this application are coherent anti-Stokes Raman scattering (CARS), laser-induced breakdown spectroscopy (LIBS), Fourier transform infrared spectroscopy (FTIR), laser-induced fluorescence (LIF), and synchronous detection of laser-induced fluorescence (SDLIF).

  13. TELCAL: The On-line Calibration Software for ALMA

    NASA Astrophysics Data System (ADS)

    Broguière, D.; Lucas, R.; Pardo, J.; Roche, J.-C.

    2011-07-01

    The ALMA on-line calibration regroups all the operations needed to maintain the ALMA interferometer optimally tuned to successfully execute the planned observations. The results of the calibrations are used in quasi-real time by the ALMA Control System. Since the first ALMA antennas were put into operation in 2009, TELCAL has been used for all the basic calibration operations and is still being improved following the project advancement. We describe here the calibrations done by TELCAL, its relationships with the other ALMA software subsystems and, briefly, the architecture of the software based on CORBA.

  14. Anisotropic alpha emission from on-line separated isotopes

    SciTech Connect

    Wouters, J.; Vandeplassche, D.; van Walle, E.; Severijns, N.; Vanneste, L.

    1986-05-05

    A systematic on-line nuclear-orientation study of heavy isotopes using anisotropic ..cap alpha.. emission is reported for the first time. The anisotrophies recorded for /sup 199/At, /sup 201/At, and /sup 203/At are remarkably pronounced and strongly varying. At lower neutron number the ..cap alpha.. particles are more preferentially emitted perpendicularly to the nuclear-spin direction. This may be interpreted in terms of the high sensitivity of the ..cap alpha..-emission probability to changes in the nuclear shape.

  15. On-line Monitoring and Active Control for Transformer Noise

    NASA Astrophysics Data System (ADS)

    Liang, Jiabi; Zhao, Tong; Tian, Chun; Wang, Xia; He, Zhenhua; Duan, Lunfeng

    This paper introduces the system for on-line monitoring and active noise control towards the transformer noise based on LabVIEW and the hardware equipment including the hardware and software. For the hardware part, it is mainly focused on the composition and the role of hardware devices, as well as the mounting location in the active noise control experiment. And the software part introduces the software flow chats, the measurement and analysis module for the sound pressure level including A, B, C weighting methods, the 1/n octave spectrum and the power spectrum, active noise control module and noise data access module.

  16. Source reduction from chemical plants using on-line optimization

    SciTech Connect

    Zhang, Z.; Pike, R.W.; Hertwig, T.A.

    1995-12-01

    An effective approach for source reduction in chemical plants has been demonstrated using on-line optimization with flowsheeting (ASPEN PLUS) for process optimization and parameter estimation and the Tjao-Biegler algorithm implemented in a mathematical programming language (GAMS/MINOS) for data reconciliation and gross error detection. Results for a Monsanto sulfuric acid plant with a Bailey distributed control system showed a 25% reduction in the sulfur dioxide emissions and a 17% improvement in the profit over the current operating conditions. Details of the methods used are described.

  17. Preparation, characterization and application of Saussurea tridactyla Sch-Bip as green adsorbents for preconcentration of rare earth elements in environmental water samples

    NASA Astrophysics Data System (ADS)

    Zhang, Qiangying; He, Man; Chen, Beibei; Hu, Bin

    2016-07-01

    This paper deals with preparation, characterization and application of the Saussurea tridactyla Sch-Bip (STSB) as a new green adsorbent for separation of matrix elements and preconcentration of rare earth elements (REEs) in environmental water samples. The pretreated STSB adsorbent with 2 mol L- 1 NaOH is characterized with higher surface area and adsorption capacities in comparison with a raw STSB material. The new adsorbent was used for the development of on-line solid phase extraction (SPE) for the determination of REEs by radial viewing 27 MHz inductively coupled plasma optical emission spectrometry (ICP-OES). Various parameters affecting the adsorption/desorption procedure were optimized. The adsorption capacities for the STSB were found to be 62.2 (Y)-153 mg g- 1 (Tm). Under the optimized conditions, the limits of detection (LODs, 3σ) for REEs were in the range of 0.06 (Yb)-8.77 (Sm) ng mL- 1. The relative standard deviations (RSDs) for 7 replicate determinations of target REEs at low concentration level ranged from 2.4 (Yb) to 8.9 (Sm)%. The adsorption isotherm fitted Langmuir model and the adsorption kinetics fitted well with both Pseudo-first order and Pseudo-second order models. The predominant adsorption mechanism is ion exchange. The STSB pretreated with 2 mol L- 1 NaOH has been demonstrated to be low cost, green and environment friendly adsorbent, featuring with high adsorption capacity, wide pH range, and fast adsorption/desorption kinetics for target REEs with long lifetime. The proposed method was applied to the determination of REEs in East Lake, Yangtze River and rain water samples.

  18. Some aspects of analytical chemistry as applied to water quality assurance techniques for reclaimed water: The potential use of X-ray fluorescence spectrometry for automated on-line fast real-time simultaneous multi-component analysis of inorganic pollutants in reclaimed water

    NASA Technical Reports Server (NTRS)

    Ling, A. C.; Macpherson, L. H.; Rey, M.

    1981-01-01

    The potential use of isotopically excited energy dispersive X-ray fluorescence (XRF) spectrometry for automated on line fast real time (5 to 15 minutes) simultaneous multicomponent (up to 20) trace (1 to 10 parts per billion) analysis of inorganic pollutants in reclaimed water was examined. Three anionic elements (chromium 6, arsenic and selenium) were studied. The inherent lack of sensitivity of XRF spectrometry for these elements mandates use of a preconcentration technique and various methods were examined, including: several direct and indirect evaporation methods; ion exchange membranes; selective and nonselective precipitation; and complexation processes. It is shown tha XRF spectrometry itself is well suited for automated on line quality assurance, and can provide a nondestructive (and thus sample storage and repeat analysis capabilities) and particularly convenient analytical method. Further, the use of an isotopically excited energy dispersive unit (50 mCi Cd-109 source) coupled with a suitable preconcentration process can provide sufficient sensitivity to achieve the current mandated minimum levels of detection without the need for high power X-ray generating tubes.

  19. On-line documentation of patient care orders.

    PubMed

    Prophet, C M

    1995-01-01

    The INFORMM NIS (Information Network For Online Retrieval & Medical Management Nursing Information System) provides on-line documentation of patient care orders. These orders, generated by the nurse or the physician, prescribe direct patient care and do not include interdepartmental orders such as laboratory, radiology, or pharmacy. The order charting functions support charting efficiency by defaulting previous responses so that the user enters only updates to earlier findings or new data. Available in tables maintained by NIS staff, charting responses provide decision support by suggesting valid results for each order. Using point-of-care devices, nursing staff chart patient data that are immediately available for review by all authorized members of the health care team. These data are printed automatically on computer-generated chart forms every twenty-four hours, but may be printed also on demand. Additionally, the patient data report, containing patient data entered on-line in the sixteen or twenty-four hours immediately preceding the print request, provides a summary that is useful for nurses' report and physicians' rounds.

  20. Characterization of optical traps using on-line estimation methods

    NASA Astrophysics Data System (ADS)

    Gorman, Jason J.; LeBrun, Thomas W.; Balijepalli, Arvind; Gagnon, Cedric; Lee, Dongjin

    2005-08-01

    System identification methods are presented for the estimation of the characteristic frequency of an optically trapped particle. These methods are more amenable to automated on-line measurements and are believed to be less prone to erroneous results compared to techniques based on thermal noise analysis. Optical tweezers have been shown to be an effective tool in measuring the complex interactions of micro-scale particles with piconewton resolution. However, the accuracy of the measurements depends heavily on knowledge of the trap stiffness and the viscous drag coefficient for the trapped particle. The most commonly referenced approach to measuring the trap stiffness is the power spectrum method, which provides the characteristic frequency for the trap based on the roll-off of the frequency response of a trapped particle excited by thermal fluctuations. However, the reliance on thermal fluctuations to excite the trapping dynamics results in a large degree of uncertainty in the estimated characteristic frequency. These issues are addressed by two parameter estimation methods which can be implemented on-line for fast trap characterization. The first is a frequency domain system identification approach which combines swept-sine frequency testing with a least-squares transfer function fitting algorithm. The second is a recursive least-squares parameter estimation scheme. The algorithms and results from simulation studies are discussed in detail.

  1. Research of on-line detection system for power capacitor

    NASA Astrophysics Data System (ADS)

    Yao, Junda; Qian, Zheng; Yu, Hao; Xia, Jiuyun

    2016-01-01

    The hidden danger exists in the power capacitor of power system due to long-time operation under the environment of high voltage. Thus, it is possible to induce serious fault, and the on-line detection system is urgently required. In this paper, two methods of the on-line detection system are compared in order to realize the better real-time condition detection. The first method is based on the STM microprocessor with an internal 12 bit A/D converter, which converts analog signals which is arrived from the sample circuit into digital signals, and then the FFT algorithm is used to accomplish the measurement of the voltage and current values of the capacitor. The second method is based on the special electric energy metering IC, which can obtain RMS (Root Mean Square) of voltage and current by processing the sampled data of the voltage and current, and store RMS of voltage and current in its certain registers. The operating condition of the capacitor can be obtained after getting the values of voltage and current. By comparing the measuring results of two methods, the second method could achieve a higher measurement accuracy and more simple construction.

  2. Polar On-Line Acquisition Relay and Transmission System (POLARATS)

    SciTech Connect

    Yuracko, K.

    2004-07-15

    POLARATS (Polar On-Line Acquisition Relay And Transmission System) is being developed by YAHSGS LLC (YAHSGS) and Oak Ridge National Laboratory (ORNL) to provide remote, unattended monitoring of environmental parameters under harsh environmental conditions. In particular, instrumental design and engineering is oriented towards protection of human health in the Arctic, and with the additional goal of advancing Arctic education and research. POLARATS will obtain and transmit environmental data from hardened monitoring devices deployed in locations important to understanding atmospheric and aquatic pollutant migration as it is biomagnified in Arctic food chains. An Internet- and personal computer (PC)-based educational module will provide real time sensor data, on-line educational content, and will be integrated with workbooks and textbooks for use in middle and high school science programs. The educational elements of POLARATS include an Internet-based educational module that will instruct students in the use of the data and how those data fit into changing Arctic environments and food chains. POLARATS will: (1) Enable students, members of the community, and scientific researchers to monitor local environmental conditions in real time over the Internet; and (2) Provide additional educational benefits through integration with middle- and high-school science curricula. Information will be relayed from POLARATS devices to classrooms and libraries along with custom-designed POLARATS teaching materials that will be integrated into existing curricula to enhance the educational benefits realized from the information obtained.

  3. On-line estimation of concentration parameters in fermentation processes.

    PubMed

    Xiong, Zhi-hua; Huang, Guo-hong; Shao, Hui-he

    2005-06-01

    It has long been thought that bioprocess, with their inherent measurement difficulties and complex dynamics, posed almost insurmountable problems to engineers. A novel software sensor is proposed to make more effective use of those measurements that are already available, which enable improvement in fermentation process control. The proposed method is based on mixtures of Gaussian processes (GP) with expectation maximization (EM) algorithm employed for parameter estimation of mixture of models. The mixture model can alleviate computational complexity of GP and also accord with changes of operating condition in fermentation processes, i.e., it would certainly be able to examine what types of process-knowledge would be most relevant for local models' specific operating points of the process and then combine them into a global one. Demonstrated by on-line estimate of yeast concentration in fermentation industry as an example, it is shown that soft sensor based state estimation is a powerful technique for both enhancing automatic control performance of biological systems and implementing on-line monitoring and optimization.

  4. On-line social interactions and executive functions

    PubMed Central

    Ybarra, Oscar; Winkielman, Piotr

    2012-01-01

    A successful social interaction often requires on-line and active construction of an ever-changing mental-model of another person’s beliefs, expectations, emotions, and desires. It also requires the ability to maintain focus, problem-solve, and flexibly pursue goals in a distraction-rich environment, as well as the ability to take-turns and inhibit inappropriate behaviors. Many of these tasks rely on executive functions (EF) – working memory, attention/cognitive control, and inhibition. Executive functioning has long been viewed as relatively static. However, starting with recent reports of successful cognitive interventions, this view is changing and now EFs are seen as much more open to both short- and long-term “training,” “warm-up,” and “exhaustion” effects. Some of the most intriguing evidence suggests that engaging in social interaction enhances performance on standard EF tests. Interestingly, the latest research indicates these EF benefits are selectively conferred by certain on-line, dynamic social interactions, which require participants to mentally engage with another person and actively construct a model of their mind. We review this literature and highlight its connection with evolutionary and cultural theories emphasizing links between intelligence and sociality. PMID:22509160

  5. On-line structure-lossless digital mammogram image compression

    NASA Astrophysics Data System (ADS)

    Wang, Jun; Huang, H. K.

    1996-04-01

    This paper proposes a novel on-line structure lossless compression method for digital mammograms during the film digitization process. The structure-lossless compression segments the breast and the background, compresses the former with a predictive lossless coding method and discards the latter. This compression scheme is carried out during the film digitization process and no additional time is required for the compression. Digital mammograms are compressed on-the-fly while they are created. During digitization, lines of scanned data are first acquired into a small temporary buffer in the scanner, then they are transferred to a large image buffer in an acquisition computer which is connected to the scanner. The compression process, running concurrently with the digitization process in the acquisition computer, constantly checks the image buffer and compresses any newly arrived data. Since compression is faster than digitization, data compression is completed as soon as digitization is finished. On-line compression during digitization does not increase overall digitizing time. Additionally, it reduces the mammogram image size by a factor of 3 to 9 with no loss of information. This algorithm has been implemented in a film digitizer. Statistics were obtained based on digitizing 46 mammograms at four sampling distances from 50 to 200 microns.

  6. Increased Cortical Thickness in Professional On-Line Gamers

    PubMed Central

    Hyun, Gi Jung; Shin, Yong Wook; Kim, Bung-Nyun; Cheong, Jae Hoon; Jin, Seong Nam

    2013-01-01

    Objective The bulk of recent studies have tested whether video games change the brain in terms of activity and cortical volume. However, such studies are limited by several factors including cross-sectional comparisons, co-morbidity, and short-term follow-up periods. In the present study, we hypothesized that cognitive flexibility and the volume of brain cortex would be correlated with the career length of on-line pro-gamers. Methods High-resolution magnetic resonance scans were acquired in twenty-three pro-gamers recruited from StarCraft pro-game teams. We measured cortical thickness in each individual using FreeSurfer and the cortical thickness was correlated with the career length and the performance of the pro-gamers. Results Career length was positively correlated with cortical thickness in three brain regions: right superior frontal gyrus, right superior parietal gyrus, and right precentral gyrus. Additionally, increased cortical thickness in the prefrontal cortex was correlated with winning rates of the pro-game league. Increased cortical thickness in the prefrontal and parietal cortices was also associated with higher performance of Wisconsin Card Sorting Test. Conclusion Our results suggest that in individuals without pathologic conditions, regular, long-term playing of on-line games is associated with volume changes in the prefrontal and parietal cortices, which are associated with cognitive flexibility. PMID:24474988

  7. Fully On-line Introductory Physics with a Lab

    NASA Astrophysics Data System (ADS)

    Schatz, Michael

    We describe the development and implementation of a college-level introductory physics (mechanics) course and laboratory that is suited for both on-campus and on-line environments. The course emphasizes a ``Your World is Your Lab'' approach whereby students first examine and capture on video (using cellphones) motion in their immediate surroundings, and then use free, open-source software both to extract data from the video and to apply physics principles to build models that describe, predict, and visualize the observations. Each student reports findings by creating a video lab report and posting it online; these video lab reports are then distributed to the rest of the class for peer review. In this talk, we will discuss the student and instructor experiences in courses offered to three distinct audiences in different venues: (1) a Massively Open On-line Course (MOOC) for off-campus participants, (2) a flipped/blended course for on-campus students, and, most recently, (3) a fully-online course for off-campus students.

  8. On-line diagnosis of sequential systems, 3

    NASA Technical Reports Server (NTRS)

    Sundstrom, R. J.

    1975-01-01

    A formal model is introduced which can serve as the basis for a theoretical investigation of on-line diagnosis. Within this model a fault of a system S is considered to be a transformation of S into another system S prime at some time tau. The resulting faulty system is taken to be the system which looks like S up to time tau and like S prime thereafter. The on-line diagnosis of systems which are structurally decomposed and represented as a network of smaller systems is also investigated. The fault set considered is the set of unrestricted component faults; namely, the set of faults which only affect one component of the network. A characterization of networks which can be diagnosed using a combinational detector is obtained. It is further shown that any network can be made diagnosable in the above sense through the addition of one component. In addition, a lower bound is obtained on the complexity of any component, the addition of which is sufficient to make a particular network combinationally diagnosable.

  9. Pulsed Neurton Elemental On-Line Material Analyzer

    DOEpatents

    Vourvopoulos, George

    2002-08-20

    An on-line material analyzer which utilizes pulsed neutron generation in order to determine the composition of material flowing through the apparatus. The on-line elemental material analyzer is based on a pulsed neutron generator. The elements in the material interact with the fast and thermal neutrons produced from the pulsed generator. Spectra of gamma-rays produced from fast neutrons interacting with elements of the material are analyzed and stored separately from spectra produced from thermal neutron reactions. Measurements of neutron activation takes place separately from the above reactions and at a distance from the neutron generator. A primary passageway allows the material to flow through at a constant rate of speed and operators to provide data corresponding to fast and thermal neutron reactions. A secondary passageway meters the material to allow for neutron activation analysis. The apparatus also has the capability to determine the density of the flowed material. Finally, the apparatus continually utilizes a neutron detector in order to normalize the yield of the gamma ray detectors and thereby automatically calibrates and adjusts the spectra data for fluctuations in neutron generation.

  10. Spectroelectrochemical Sensor for Technetium: Preconcentration and Quantification of Technetium in Polymer Modified Electrodes

    SciTech Connect

    Monk, David J.; Stegemiller, Michael L.; Conklin, Sean; Paddock, Jean R.; Heineman, William R.; Seliskar, Carl J.; Ridgway, Thomas H.; Bryan, Samuel A.; Hubler, Tim L.

    2003-03-27

    A remote spectroelectrochemical sensor and instrumentation package is being developed for the detection of aqueous pertechnetate in the vadose zone. This sensor can be employed to monitor the integrity of low-level and high-level nuclear waste containment at U.S. DOE sites. A brief review of previous advancements and current development of this sensor is described. Initial spectroelectrochemical studies of pertechnetate using unmodified and polymer modified optically transparent electrodes have shown that the polymer modified electrode will readily preconcentrate pertechnetate. The electrodeposition of technetium oxide in these films is shown to be a method for the quantitative spectroelectrochemical determination of technetium and has been verified using radiochemistry dose measurements and scanning electron microscopy. The irreversible electrochemical nature of pertechnetate in polymer modified electrodes demonstrates the need to identify a ligand capable of complexing wi th technetium, to allow reversible detection and to provide additional chemical selectivity.

  11. Analysis of alkyl nitrates and selected halocarbons in the ambient atmosphere using a charcoal preconcentration technique

    SciTech Connect

    Atlas, E.; Schauffler, S. )

    1991-01-01

    A method has been developed to measure {ge}C{sub 3} alkyl nitrates and C{sub 1}-C{sub 2} halocarbons, such as perchloroethylene and bromoform, in ambient air. The method preconcentrates analytes on a 5-mg charcoal trap from multiliter volumes of air. Analytes are desorbed from the charcoal with a small volume of solvent and are analyzed by high-resolution gas chromatography with electron capture detection. Laboratory and field tests have been performed to evaluate method precision, analyte breakthrough, and compound recovery from the charcoal. Tests verified that the sampling/analytical system is free from artifact formation under clean to moderately polluted conditions, but further tests are required for areas of high concentrations of hydrocarbons, NO{sub x}, and oxidants. The method allows measurement of halocarbons and {ge}C{sub 3} alkyl nitrates at concentrations in the pptv range.

  12. Column preconcentration and faas determination of heavy metal ions using Artemisia Siberi as an adsorbent.

    PubMed

    Mousavi, Hassan Zavvar; Derakhshankhah, Jalal

    2014-01-01

    A new column procedure for the determination of trace amounts of cadmium (II), lead (II), nickel (II), zinc (II), and copper (II), which combines flame atomic absorption spectrometry is described. These metals were sorbed on Artemisia siberi herb as an adsorbent at pH 4.0 and eluted with 3 mL of 1.5 M HNO3. The influences of analytical parameters including pH, flow rate, sample volume, type of eluent, and effect of diverse salts and cations on the recoveries of analyte ions were studied. The developed procedure provides preconcentration factors of about 117. LODs were 0.2 (Cd), 0.4 (Cu), 0.2 (Ni), 0.6 (Zn), and 1.4 (Pb) μg/L. The present method was successfully applied to the determination of the above-mentioned ions in water samples from Semnan, Iran. Recoveries greater than 95% and RSDs below 10% were obtained. PMID:25632447

  13. Mass-spectrometric determination of trace elements in aqueous media without preconcentration

    SciTech Connect

    Foss, G. O.

    1981-10-01

    Feasibility of using a low pressure glow discharge as an ion source for the mass spectrometric determination of trace elements in aqueous media was investigated. A cryogenically cooled hollow cathode ion source was developed to analyze aqueous samples without external preconcentration. Aqueous solutions containing seventy elements were analyzed and the detection limits, sensitivity factors, and linear regression correlation coefficients were determined. A standard test solution of trace elements in water was analyzed and the concentrations of trace elements were calculated using the sensitivity factors determined previously. The results compared favorably within the error limits predicted by the semiquantitative survey methods used. Tap water and natural lake water samples were examined and minimal interference effects due to organic compounds and biological compounds were noted. A research ion optical system (RIOS) was developed as a flexible mass analyzer for the development of new ion sources. The RIOS is a double focussing mass analyzer designed utilizing the Mattauch-Herzog geometry with externally adjustable slit assemblies.

  14. Cloud point extraction, preconcentration and simultaneous spectrophotometric determination of nickel and cobalt in water samples

    NASA Astrophysics Data System (ADS)

    Safavi, A.; Abdollahi, H.; Hormozi Nezhad, M. R.; Kamali, R.

    2004-10-01

    Cloud point extraction has been used for the preconcentration and simultaneous spectrophotometric determination of nickel and cobalt after the formation of a complex with 2-amino-cyclopentene-1-dithiocarboxylic acid (ACDA), and latter analysis by spectrophotometer using Triton X-114 as surfactant. The parameters affecting the separation phase and detection process were optimized. Under the optimum experimental conditions (i.e. pH=5, 0.07 mM ACDA, Triton X-114 = 0.25% (w/v)), calibration graphs were linear in the range of 20-500 and 20-200 μg l -1 with detection limits of 10 and 7.5 μg l -1 for Ni and Co, respectively. The method was applied to the determination of Ni and Co in natural and waste water samples with satisfactory results.

  15. Magnetic nanoparticles as sorbent for preconcentration and determination of lead in fish and water samples

    NASA Astrophysics Data System (ADS)

    Khajeh, M.; Sanchooli, E.

    2011-07-01

    In the present work, a procedure for the preconcentration and determination of lead trace amounts of lead in fish species and water samples by graphite furnace atomic absorption spectrometry (GF AAS) is proposed, which is based on the batch solid phase extraction of lead ions by modified magnetic nanoparticles. An optimization process was performed using two-level fractional factorial designs (24-1) and a Box-Behnken matrix. Four variables (pH of solution, nanoparticles mass, morin mass, and shaking time) were regarded as factors in the optimization. The detection limit of the proposed method was found to be 81.0 ng/l. Six samples of fish and three samples of water (tap, river, and lake) were analyzed for lead. The lead contents ranged in fish from 0.013 to 0.038 μg/g and in water from 7.1 to 9.0 μg/l.

  16. FEDIX on-line information service: Design, develop, test, and implement, an on-line research and education information service

    SciTech Connect

    Rodman, J.A.

    1992-01-01

    The FEDIX Annual Status Report provides details regarding an on-line information project designed, developed and implemented by Federal Information Exchange, Inc., a diversified information services company. This document details the project design activities, summarizes the developmental phases of the project and describes the implementation activities generated to fulfill the project's objectives. The information contained in this document illustrates FIE's continuing commitment to serve as the link that facilitates the dissemination of federal information to the education community. This report reviews the project accomplishments and describes intended service enhancements.

  17. Selenium Preconcentration in Geological Materials for Determination at sub-μ g\\ g-1 Concentration

    NASA Astrophysics Data System (ADS)

    Bedard, L. P.

    2004-05-01

    Selenium is important because it is a path finder element in economic geology. It has similar geochemical properties as sulfur, but slightly less mobile and less volatile in sulfides. Although its environmental cycle is better understood, its geological cycle is almost unknown. In geological samples, Se concentration ranges 0,02-1 μ g\\ g-1. Se has many spectral interefences in ICP-MS, rendering difficult to determine. INAA detection limit for geological samples is about 10 μ g\\ g-1. The analytical difficulties are one of the main reason why the geological cycle of Se is so poorly known. The preconcentration of Se with Thiol Cotton Fiber (TCF) followed by atomic absorption (AA) has been modified to be used with INAA. The modified technique involves sample dissolution (HF-HNO3) and evaporation to dryness at low temperature (55-60 oC) to keep Se in solution. Se is converted to SeIV by adding 5-6 mol l-1 HCl and heating covered in a boiling bath (95-100oC). Sample is diluted with deionized water to obtain 0,3 - 1 mol l-1 HCl and then collected on TCF. TCF is put in a polyethylene vial for irradiation in the SLOWPOKE II reactor for 10 seconds at a neutron flux of 1015 m-2 s-1. The 162 KeV peak of 77Se (half-life 17,36 sec) is read for 20 seconds after a decay of 7 seconds. Results for certified reference materials show the TCF preconcentration technique followed by INAA provides results comparable with AA with a detection limit of approximately 0,05 μ g\\ g-1. Moreover INAA provides many advantages such as eliminating the desorption step and is less time consuming than AA.

  18. Integrated continuous flow polymerase chain reaction and micro-capillary electrophoresis system with bioaffinity preconcentration.

    PubMed

    Njoroge, Samuel K; Witek, Magorzata A; Battle, Katrina N; Immethun, Vicki E; Hupert, Mateusz L; Soper, Steven A

    2011-11-01

    An integrated and modular DNA analysis system is reported that consists of two modules: (i) A continuous flow polymerase chain reaction (CFPCR) module fabricated in a high T(g) (150°C) polycarbonate substrate in which selected gene fragments were amplified using biotin and fluorescently labeled primers accomplished by continuously shuttling small packets of PCR reagents and template through isothermal zones as opposed to heating and cooling large thermal masses typically performed in batch-type thermal reactors. (ii) μCE (micro-capillary electrophoresis) module fabricated in poly(methylmethacrylate) (PMMA), which utilized a bioaffinity selection and purification bed (2.9  μL) to preconcentrate and purify the PCR products generated from the CFPCR module prior to electrophoretic sorting. Biotin-labeled CFPCR products were hydrostatically pumped through the streptavidin-modified bed, where they were extracted onto the surface of micropillars. The affinity bed was also fabricated in PMMA and was populated with an array of microposts (50  μm width; 100  μm height) yielding a total surface area of ∼117  mm(2). This solid-phase extraction (SPE) process demonstrated high selectivity for biotinylated amplicons and utilized the strong streptavidin/biotin interaction (K(d) = 10(-15)  M) to generate high recoveries. The SPE selected CFPCR products were thermally denatured and single-stranded DNA released for injection into a 7-cm-long μCE channel for size-based separations and fluorescence detection. The utility of the system was demonstrated using Alu DNA typing for gender and ethnicity determinations as a model. Compared with the traditional cross-T injection procedure typically used for μCE, the affinity pre-concentration and injection procedure generated signal enhancements of 17- to 40-fold, critical for CFPCR thermal cyclers due to Taylor dispersion associated with their operation. PMID:22038569

  19. Evaluation of functionalized isoreticular metal organic frameworks (IRMOFs) as smart nanoporous preconcentrators of RDX

    SciTech Connect

    Xiong, Ruichang; Odbadrakh, Khorgolkhuu; Michalkova, Andrea; Luna, Johnathan P.; Petrova, Tetyana; Keffer, David J.; Nicholson, Don M; Fuentes-Cabrera, Miguel A; Lewis, James; Leszczynski, Jerzy

    2010-01-01

    Classical molecular dynamics (MD) and Grand Canonical Monte Carlo (GCMC) simulations were used to generate self-diffusivities, adsorption isotherms and density distributions for hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in five isoreticular metal-organic frameworks (IRMOFs), which varied in the cage size and in the presence and location of amine groups. These simulations were performed at room temperature (300 K) and low pressures (up to 1 ppm RDX). The atomic charges required for MD and GCMC simulations were calculated from quantum mechanical (QM) calculations using two different charge generation methods - Loewdin Population Analysis and Natural Bond Orbital Analysis. Both charge sets show that the presence of amine groups increases the amount of RDX adsorbed. The cage size and the location of amine groups also affect the loading of RDX. The amount of RDX adsorbed is correlated with the energy of adsorption. The activation energy for diffusion of RDX is not positively correlated with the energy of adsorption. The density distributions identify the location of the adsorption sites of RDX-exclusively in the big cage around the metal complex vertices and between benzene rings. In the absence of amine groups on the framework, one of nitro groups on RDX interacts closely with the metal complex. In the IRMOFs functionalized with amine groups, a second nitro group of the RDX interacts with an amine group, enhancing adsorption. With regard to the application as a smart nanoporous preconcentrator, these IRMOFs are found to concentrate RDX up to 3000 times compared to the gas phase, on a volumetric basis. From a simple Langmuir estimation, the selectivity of RDX over butane is up to 5000. The diffusion of RDX is sufficiently high for real time sensor applications. These results indicate IRMOFs can be tailored with functional groups to be highly selective nanoporous preconcentrators.

  20. On-line analysis of secondary ozonides from cyclohexene and D-limonene ozonolysis using atmospheric sampling townsend discharge ionization mass spectrometry

    NASA Astrophysics Data System (ADS)

    Nøjgaard, J. K.; Nørgaard, A. W.; Wolkoff, P.

    An on-line technique has been developed for analysis of gas-phase oxidation products formed in a reaction flow tube using different reaction times, concentrations and humidities. Products of ozonolysis, including thermally labile secondary ozonides (SOZ), were directly introduced into an atmospheric sampling townsend discharge ionization (ASTDI) source coupled to a triple quadrupole mass spectrometer (MS). Instant changes in the product composition were monitored in the total-ion chromatogram, or by fragment ions in the collision activated dissociation mass spectra by use of MS/MS scan techniques. Assignment of the individual ions was accomplished by inspection of the products' mass spectra obtained by pre-concentration of the gas phase on a dedicated short column followed by chromatographic analysis. The observed reaction products correspond to those identified with other techniques. Of relevance for future mechanistic modelling, is the point that conditions of excess D-limonene favoured the formation of the D-limonene SOZ (major product), which was observed to be quite stable in dry and humid air, without oxidants. The D-limonene/ozone ratio was observed to be crucial for the stability of the SOZ, because it is prone to ozonolysis, and no SOZ could be detected in completely reacted 1:1 mixtures.

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

    PubMed

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

    2014-12-01

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

  2. On-line sample processing involving microextraction techniques as a front-end to atomic spectrometric detection for trace metal assays: a review.

    PubMed

    Miró, Manuel; Hansen, Elo Harald

    2013-06-11

    Within the last decade, liquid-phase microextraction (LPME) and micro-solid phase extraction (μSPE) approaches have emerged as substitutes for conventional sample processing procedures for trace metal assays within the framework of green chemistry. This review surveys the progress of the state of the art in simplification and automation of microextraction approaches by harnessing to the various generations of flow injection (FI) as a front end to atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS) or inductively coupled plasma atomic emission spectrometry or mass spectrometry (ICP-AES/MS). It highlights the evolution of flow injection analysis and related techniques as vehicles for appropriate sample presentation to the detector and expedient on-line matrix separation and pre-concentration of trace levels of metals in troublesome matrices. Rather than being comprehensive this review is aimed at outlining the pros and cons via representative examples of recent attempts in automating green sample preparation procedures in an FI or sequential injection (SI) mode capitalizing on single-drop microextraction, dispersive liquid-phase microextraction and advanced sorptive materials including carbon and metal oxide nanoparticles, ion imprinted polymers, superparamagnetic nanomaterials and biological/biomass sorbents. Current challenges in the field are identified and the synergetic combination of flow analysis, nanotechnology and metal-tagged biomolecule detection is envisaged. PMID:23708278

  3. Electroplating of nanostructured polyaniline-polypyrrole composite coating in a stainless-steel tube for on-line in-tube solid phase microextraction.

    PubMed

    Asiabi, Hamid; Yamini, Yadollah; Seidi, Shahram; Esrafili, Ali; Rezaei, Fatemeh

    2015-06-01

    In this work, a novel and efficient on-line in-tube solid phase microextraction method followed by high performance liquid chromatography was developed for preconcentration and determination of trace amounts of parabens. A nanostructured polyaniline-polypyrrole composite was electrochemically deposited on the inner surface of a stainless steel tube and used as the extraction phase. Several important factors that influence the extraction efficiency, including type of solid-phase coating, extraction and desorption times, flow rates of the sample solution and eluent, pH, and ionic strength of the sample solution were investigated and optimized. Under the optimal conditions, the limits of detection were in the range of 0.02-0.04 μg L(-1). This method showed good linearity for parabens in the range of 0.07-50 μg L(-1), with coefficients of determination better than 0.998. The intra- and inter-assay precisions (RSD%, n=3) were in the range of 5.9-7.0% and 4.4-5.7% at three concentration levels of 2, 10, and 20 μg L(-1), respectively. The extraction recovery values for the spiked samples were in the acceptable range of 80.3-90.2%. The validated method was successfully applied for analysis of methyl-, ethyl-, and propyl parabens in some water, milk, and juice samples.

  4. Automated microextraction sample preparation coupled on-line to FT-ICR-MS: application to desalting and concentration of river and marine dissolved organic matter.

    PubMed

    Morales-Cid, Gabriel; Gebefugi, Istvan; Kanawati, Basem; Harir, Mourad; Hertkorn, Norbert; Rosselló-Mora, Ramón; Schmitt-Kopplin, Philippe

    2009-10-01

    Sample preparation procedures are in most cases sample- and time-consuming and commonly require the use of a large amount of solvents. Automation in this regard can optimize the minimal-needed injection volume and the solvent consumption will be efficiently reduced. A new fully automated sample desalting and pre-concentration technique employing microextraction by packed sorbents (MEPS) cartridges is implemented and coupled to an ion cyclotron resonance Fourier-transform mass spectrometer (ICR-FT/MS). The performance of non-target mass spectrometric analysis is compared for the automated versus off-line sample preparation for several samples of aqueous natural organic matter. This approach can be generalized for any metabolite profiling or metabolome analysis of biological materials but was optimized herein using a well characterized but highly complex organic mixture: a surface water and its well-characterized natural organic matter and a marine sample having a highly salt charge and enabling to validate the presented automatic system for salty samples. The analysis of Suwannee River water showed selective C18-MEPS enrichment of chemical signatures with average H/C and O/C elemental ratios and loss of both highly polar and highly aromatic structures from the original sample. Automated on-line application to marine samples showed desalting and different chemical signatures from surface to bottom water. Relative comparison of structural footprints with the C18-concentration/desalting procedure however enabled to demonstrate that the surface water film was more concentrated in surface-active components of natural (fatty acids) and anthropogenic origin (sulfur-containing surfactants). Overall, the relative standard deviation distribution in terms of peak intensity was improved by automating the proposed on-line method. PMID:19685041

  5. Optical instrumentation for on-line analysis of chemical processes

    SciTech Connect

    Hartford, A. Jr.; Cremers, D.A.; Loree, T.R.; Quigley, G.P.

    1983-01-01

    Optical diagnostics provide the capability for nonintrusive, on-line, real time analysis of chemical process streams. Several laser-based methods for monitoring fossil energy processes have been evaluated. Among the instrumentation techniques which appear quite promising are coherent anti-Stokes Raman spectroscopy (CARS), laser-induced breakdown spectroscopy (LIBS), and synchronous detection of laser-induced fluorescence (SDLIF). A CARS diagnostic was implemented on a coal gasifier and was successfully employed to measure species concentrations and temperatures within the process stream. The LIBS approach has been used to identify total trace impurities (e.g., Na, K, and S) within a gasifier. Recently, individual components in mixtures of aromatics hydrocarbons have been resolved via the synchronous detection of laser-induced fluorescence. 9 figures.

  6. WMI2, the student's on-line symbolic calculator

    NASA Astrophysics Data System (ADS)

    Kovács, Zoltán

    2011-06-01

    Student activities focused on discovering mathematics play an important role in the teaching and learning process. WebMathematics Interactive (WMI2) was developed to offer a fast and user-friendly on-line web interface to enhance the quality of both theoretical and applied mathematics courses. For the teacher, in the classroom, it provides immediate numerical computations, algebraic manipulations and graphical representations. For our students, WMI2 provides a unique classroom experience in their own Hungarian language that generates various mathematical representations. At home our students have a support system to help them explore mathematical concepts, test their mathematical knowledge and to assist them in their problem solving. WMI2 has been under continuous development since 2002 and has been in classroom use since 2007. It is freely available in 10 languages.

  7. PHEBUS on-line aerosol monitor development test program

    SciTech Connect

    Sprenger, M.H.; Pentecost, C.G.

    1992-03-01

    EG&G Idaho, Inc. developed an on-line aerosol monitor (OLAM) for the French PHEBUS Fission Product Project. Part of the development was to manufacture and test an OLAM prototype. This report presents the results of the testing which determined the mechanical integrity of the monitor at operating temperature and pressure and performed a preliminary test of the optical system. A series of twenty different tests was conducted during the prototype testing sequence. Since no leaks were detected, the OLAM demonstrated that it could provide a pressure boundary at required test conditions. The optical and electrical system also proved its integrity by exceeding the design requirement of less than 105 optical signal drift during an actual two-hour test sequence.

  8. PHEBUS on-line aerosol monitor development test program

    SciTech Connect

    Sprenger, M.H.; Pentecost, C.G.

    1992-03-01

    EG G Idaho, Inc. developed an on-line aerosol monitor (OLAM) for the French PHEBUS Fission Product Project. Part of the development was to manufacture and test an OLAM prototype. This report presents the results of the testing which determined the mechanical integrity of the monitor at operating temperature and pressure and performed a preliminary test of the optical system. A series of twenty different tests was conducted during the prototype testing sequence. Since no leaks were detected, the OLAM demonstrated that it could provide a pressure boundary at required test conditions. The optical and electrical system also proved its integrity by exceeding the design requirement of less than 105 optical signal drift during an actual two-hour test sequence.

  9. On-line data acquisition using a multiprocessor architecture

    SciTech Connect

    DeAsmundis, R.; Spadaccini, G.; Terrasi, F. )

    1989-10-01

    In this paper a system for on-line data processing based on a multiprocessor architecture and a PC/AT is presented. Many improvements with respect to a previous published architecture have been introduced in order to speed-up the processing and the display features of the system. A new CAMAC module for event identification and triggering has been designed and assembled. Collected data are now recorded on a magnetic tape unit, and integrated data (1-dim. and 2-dim. spectra) are handled by a PC/AT linked directly to the system. Although almost the whole code is stored in Eprom, the PC/AT supports also mass-storage and development features for debug phases of the system software.

  10. On-line detection of human skin vapors.

    PubMed

    Martínez-Lozano, Pablo; de la Mora, Juan Fernández

    2009-06-01

    Vapors released by the skin in the hand of one human subject are detected in real time by sampling them directly from the ambient gas surrounding the hand, ionizing them by secondary electrospray ionization (SESI, via contact with the charged cloud from an electrospray source), and analyzing them in a mass spectrometer with an atmospheric pressure source (API-MS). This gas-phase approach is complementary to alternative on-line surface ionization methods such as DESI and DART. A dominating peak of lactic acid and a complete series of saturated and singly unsaturated fatty acids (C(12) to C(18)) are observed, in accordance with previous off-line studies by gas chromatography-mass spectrometry. Several other metabolites have been identified, including ketomonocarboxylic and hydroxymonocarboxylic acids.

  11. Synthetic Gene Design Using Codon Optimization On-Line (COOL).

    PubMed

    Yu, Kai; Ang, Kok Siong; Lee, Dong-Yup

    2017-01-01

    Codon optimization has been widely used for designing native or synthetic genes to enhance their expression in heterologous host organisms. We recently developed Codon Optimization On-Line (COOL) which is a web-based tool to provide multi-objective codon optimization functionality for synthetic gene design. COOL provides a simple and flexible interface for customizing codon optimization based on several design parameters such as individual codon usage, codon pairing, and codon adaptation index. User-defined sequences can also be compared against the COOL optimized ones to show the extent by which the user's sequences can be evaluated and further improved. The utility of COOL is demonstrated via a case study where the codon optimized sequence of an invertase enzyme is generated for the enhanced expression in E. coli. PMID:27671929

  12. Issues for Bringing Electron Beam Irradiators On-Line

    SciTech Connect

    Kaye, R.J.; Turman, B.N.

    1999-04-20

    Irradiation of red meat and poultry has been approved by the U.S. FDA, and the U.S. Department of Agriculture's rule for processing red meat is out for comment. Looking beyond the current issues of packaging materials, labeling, and consumer acceptance, this paper reviews the next step of implementation and how to remove, or at least reduce, the barriers to utilization. Polls of the user community identified their requirements for electron beam or x-ray processing of meat or poultry and their concerns about implementation for on-line processing. These needs and issues are compared to the capabilities of the accelerator industry. The critical issues of beam utilization and dose uniformity, factors affecting floor space requirements, and treatment costs are examined.

  13. SBR on-line monitoring by set-point titration.

    PubMed

    Fiocchi, N; Ficara, E; Canziani, R; Luccarini, L; Ciappelloni, F; Ratini, P; Pirani, M; Mariani, S

    2006-01-01

    The applicability of set-point titration for monitoring biological processes has been widely demonstrated in the literature. Based on published and on-going experiences, some operating procedures have been specifically developed to be applied to SBRs, so that real-time information about the process and/or the influent can be obtained. This, in turn, would allow plant operators to select the most appropriate actions properly and timely. Five operating modes are described for the monitoring of (1) influent toxicity, (2) influent N-content, (3) nitrification capacity, (4) end of the nitrification reaction, and (5) nitrate effluent concentration, and are currently tested on the on-line titrator TITAAN (TITrimetric Automated ANalyser) which is in operation on a pilot scale SBR. PMID:16722107

  14. Children's on-line processing of scrambling in Japanese.

    PubMed

    Suzuki, Takaaki

    2013-04-01

    This study investigates the on-line processing of scrambled sentences in Japanese by preschool children and adults using a combination of self-paced listening and speeded picture selection tasks. The effects of a filler-gap dependency, reversibility, and case markers were examined. The results show that both children and adults had difficulty in comprehending scrambled sentences when they were provided as reversible sentences. The reversibility effect was significant for children, whereas the interaction of reversibility and a filler-gap dependency was significant for adults. However, this does not indicate that children's parsing is fundamentally different from that of adults. For those children who processed the nominative and accusative case markers equally fast, the reactivation of the dislocated constituent was observed in the gap position. These results suggest that children's processing is basically the same as adults' in that their sentence processing is incremental and they parse a gap to form a filler-gap dependency. PMID:22460686

  15. Memphis Area Rideshare on-line information system

    SciTech Connect

    Not Available

    1984-02-01

    Since the mid 1970s, there has been an evolution in data processing needs at regional ridesharing agencies. Initially, ridesharing programs were basically ''areawide carpooling efforts'' which stressed pre-planned commuter surveys and large-scale computerized carpool matching using batch mode procedures. However, experience gained in efforts to influence urban travel behavior has led to the adoption of comprehensive marketing strategies and personalized transportation brokerage techniques which are more responsive to commuter needs. With this changing emphasis, new data processing tools are needed which will support new ridesharing marketing strategies, not dictate them. As described in this report, the method taken at Memphis Area Rideshare to acquire data processing capabilities needed to support new marketing approaches involved development of an in-house, on-line multi-user system using POOLMATCH ridesharing software.

  16. On-Line Robust Modal Stability Prediction using Wavelet Processing

    NASA Technical Reports Server (NTRS)

    Brenner, Martin J.; Lind, Rick

    1998-01-01

    Wavelet analysis for filtering and system identification has been used to improve the estimation of aeroservoelastic stability margins. The conservatism of the robust stability margins is reduced with parametric and nonparametric time- frequency analysis of flight data in the model validation process. Nonparametric wavelet processing of data is used to reduce the effects of external disturbances and unmodeled dynamics. Parametric estimates of modal stability are also extracted using the wavelet transform. Computation of robust stability margins for stability boundary prediction depends on uncertainty descriptions derived from the data for model validation. The F-18 High Alpha Research Vehicle aeroservoelastic flight test data demonstrates improved robust stability prediction by extension of the stability boundary beyond the flight regime. Guidelines and computation times are presented to show the efficiency and practical aspects of these procedures for on-line implementation. Feasibility of the method is shown for processing flight data from time- varying nonstationary test points.

  17. On-Line Safe Flight Envelope Determination for Impaired Aircraft

    NASA Technical Reports Server (NTRS)

    Lombaerts, Thomas; Schuet, Stefan; Acosta, Diana; Kaneshige, John

    2015-01-01

    The design and simulation of an on-line algorithm which estimates the safe maneuvering envelope of aircraft is discussed in this paper. The trim envelope is estimated using probabilistic methods and efficient high-fidelity model based computations of attainable equilibrium sets. From this trim envelope, a robust reachability analysis provides the maneuverability limitations of the aircraft through an optimal control formulation. Both envelope limits are presented to the flight crew on the primary flight display. In the results section, scenarios are considered where this adaptive algorithm is capable of computing online changes to the maneuvering envelope due to impairment. Furthermore, corresponding updates to display features on the primary flight display are provided to potentially inform the flight crew of safety critical envelope alterations caused by the impairment.

  18. An on-line calibration method for process gas chromatographs

    SciTech Connect

    Fang, M.; Wang, F.

    1995-05-01

    Gas chromatographs (GCs) used to measure gas concentrations in process streams usually need calibration for a wide range of concentrations. The gas chromatographs used in process applications are usually equipped with automatic samplers using sample loops. The sampling system can be modified to provide on-line calibration, by adding a vacuum system and a precision pressure gage. In this paper, the authors describe a method using pure gases for the calibration of automatic GCs by varying and measuring precisely the pressure of the sample loop, thus sending known quantities of gas into the column. The concentration of the gas is calculated using the ideal gas law, and they are able to calibrate GCs in a range from 1,000 ppm to 100 vol %.

  19. On-line control of the nonlinear dynamics for synchrotrons

    NASA Astrophysics Data System (ADS)

    Bengtsson, J.; Martin, I. P. S.; Rowland, J. H.; Bartolini, R.

    2015-07-01

    We propose a simple approach to the on-line control of the nonlinear dynamics in storage rings, based on compensation of the nonlinear resonance driving terms using beam losses as the main indicator of the strength of a resonance. The correction scheme is built on the analysis of the resonance driving terms in first perturbative order and on the possibility of using independent power supplies in the sextupole magnets, which is nowadays present in many synchrotron light sources. Such freedom allows the definition of "smart sextupole knobs" attacking each resonance separately. The compensation scheme has been tested at the Diamond light source and proved to be effective in opening up the betatron tune space, resonance free, available to the electron beam and to improve the beam lifetime.

  20. State of the art in on-line techniques coupled to flow injection analysis FIA/on-line- a critical review

    PubMed Central

    Puchades, R.; Maquieira, A.; Atienza, J.; Herrero, M. A.

    1990-01-01

    Flow injection analysis (FIA) has emerged as an increasingly used laboratory tool in chemical analysis. Employment of the technique for on-line sample treatment and on-line measurement in chemical process control is a growing trend. This article reviews the recent applications of FlA. Most papers refer to on-line sample treatment. Although FIA is very well suited to continuous on-line process monitoring, few examples have been found in this areamost of them have been applied to water treatment or fermentation processes. PMID:18925271

  1. On-site solid-phase extraction and application to in situ preconcentration of heavy metals in surface water.

    PubMed

    Jiao, Fang; Gao, Hong-Wen

    2013-01-01

    An on-site solid-phase extraction, consisting of the sorption, the separation and the elution function units, was designed for in situ preconcentration of heavy metals ions. The D401 resin powder was employed as sorbent to capture Pb(2+), Cu(2+), Zn(2+), Cd(2+), Co(2+), and Ni(2+), and then they desorbed with 2 mol/L nitric acid as eluent. Under the optimized conditions, these heavy metals ions in West Lake, Taihu Lake, and Yangtze River of China were captured and then determined by ICP-OES with the recovery of 92.5% to 111.5%. The on-site solid-phase extraction achieved a quick preconcentration of heavy metals to avoid the transport and storage of a large volume water sample. It is suitable for in situ monitoring of water quality in mountains, tablelands or other remote areas. PMID:22286838

  2. Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

    PubMed

    Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

    2013-12-01

    A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results.

  3. Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

    PubMed

    Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

    2013-12-01

    A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results. PMID:25078838

  4. The determination of ozone precursors with a built-in preconcentrator and capillary GC/dual FID

    SciTech Connect

    Kirshen, N.; Coe, D.

    1994-12-31

    Title 1 of the Clean Air Act Amendments of 1990 requires cities or air quality districts that are non-compliant with the Ozone National Ambient Air Quality Standard of 120 ppbv to make continuous measurements of targeted ozone precursors. Air samples must be obtained on a one to three hour basis with the requirement that a high percentage of the time interval will be spent in the sample collection process. The preconcentration of the target analytes from these samples by absorbent trapping rather than the traditional use of cryogenic preconcentration on glass beads with liquid nitrogen has been utilized over the past few years for this application. An Ozone Precursor GC system has been configured with a new built-in sample preconcentration trap (SPT) and associated valving capable of preconcentrating a 200 mL air sample. The sample which may be drawn either from a canister or directly from the ambient air first passes through a stripper column for moisture removal and then through an adsorbent trap. The adsorbent trap is cooled to initial conditions with a very small amount of liquid carbon dioxide providing many runs from one cylinder. Following trapping, the precursors are quickly desorbed with the fast heating (40 C/sec) SPT to parallel columns of Alumina Plot and DB-1 for chromatographic separation and quantitation of the trapped analytes. Dual FIDs provide detection. Optimization of the trapping and chromatographic parameters has been performed using a 60 component EPA precursor standard. The results of these studies and a description of the integrated system will be presented.

  5. Determination of platinum and palladium in geological materials by neutron-activation analysis after fire-assay preconcentration

    USGS Publications Warehouse

    Rowe, J.J.; Simon, F.O.

    1971-01-01

    Fire-asay preconcentration followed by neutron-activation analysis permits the determination of as little as 0.5 ppM of platinum and 0.5 ppM of palladium on a 20-g sample. Platinum and palladium are separated with carriers and beta-counted. Results for the platinum and palladium content of seven U.S.G.S. standard rocks are presented. ?? 1971.

  6. On-line sterilization of cheese whey using ultraviolet radiation.

    PubMed

    Mahmoud, N S; Ghaly, A E

    2004-01-01

    The effectiveness of ultraviolet radiation for on-line sterilization of cheese whey was investigated. The effects of flow rate and residence time on the performance of three UV reactors having different gap sizes (18, 13, and 6 mm) were studied. Six flow rates and six residence times were tested with the three UV reactors. The cheese whey used in this study had a very high turbidity (4317 NTU), very poor transmittance in the UV radiation germicidal range ( approximately 0%), and high percentage of large solid particles ( approximately 20% > 100 microm). Although the cheese whey physical characteristics showed low probability of sterilization using UV radiation, the study showed that UV radiation can be used on-line to sterilize cheese whey if the proper reactor gap size and the appropriate residence time are used. There were combined effects of the flow rate and gap size. The cell removal efficiency increased with increases in residence time and decreases in the UV reactor gap size. Removal efficiency of 100% was not achieved in this study with the first UV reactor (18-mm gap size), whereas 100% removal efficiency was achieved with the second (13-mm gap size) and third (6-mm gap size) UV reactors at residence times of 2.0 and 0.5 h, respectively. The microbial decay rates achieved in this study were 4.94, 7.62, and 20.9 h(-)(1) using the first, second, and third UV reactor, respectively. Residence times of 3.3, 2.1, and 0.8 h would be required to completely destruct a microbial population of 5.95 x 10(6) cells/mL using the first, second, and third UV reactors, respectively. Although cheese whey sterilization using UV radiation seems to be a good alternative to pasteurization, increases in cheese whey temperature resulted in lamp fouling. If online sterilization is to be used, the fouling problem should be investigated and a maintenance scheme for the UV reactor should be developed.

  7. On-line tool misalignment detection using an imaging method

    NASA Astrophysics Data System (ADS)

    Xie, Tong

    The Opticam spherical surface generator is developed at the Center for Optics Manufacturing (COM). It combines computer-numerical-control (CNC) technology with bound abrasive ring grinding geometry to create advantages over the conventional loose abrasive grinding systems in flexibility, productivity and accuracy. The Opticam SX utilizes a ring grinding geometry to generate spherical surfaces. By adjusting the tilt angle and the diameter of the ring cutter, the Opticam is capable of generating spherical surfaces with an essentially unlimited range of radius of curvature. This ring grinding geometry, however, requires a precise alignment between the cutter and the generated part. Residual cutter misalignments in the machine setup cause the finished surface to deviate from the design shape. Current tool misalignment detection techniques seriously limit the productivity of the Opticam system, and a new metrology system is introduced in this dissertation. The new system is geometrical ray trace based, and has some similarities to the moire deflectometry techniques. It uses a non-contact method to measure surface slope errors from images reflected off Opticam generated surfaces. The detected slope errors are used to determine the corresponding tool misalignments in the Opticam generator. The system setup is simple and not sensitive to vibrations. This system is compatible with the wet grinding environment. Furthermore, this new metrology system is capable of measuring surfaces with a wide range of radius of curvature from convex to concave. A prototype system was built based on this technique. It has been evaluated on-line in the Opticam SX. A surface wetting technique is used to allow detection on Opticam generated surfaces independent of the actual surface finish. The experimental results suggested that the on- line detection system is capable of detecting tool misalignment corresponding to a peak-to-valley surface figure error that is 1 μm or greater on ground

  8. Stress Caused by On-Line Collaboration in E-Learning: A Developing Model

    ERIC Educational Resources Information Center

    Allan, John; Lawless, Naomi

    2003-01-01

    On-line collaboration is becoming increasingly common in education and in organisations. It was believed that this could in itself cause stress for collaborators. An analysis of on-line learning diaries, phone interviews and questionnaires indicated that on-line collaboration could cause stress, and this stress was linked to the dependency of the…

  9. 21 CFR 870.4330 - Cardiopulmonary bypass on-line blood gas monitor.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Cardiopulmonary bypass on-line blood gas monitor. 870.4330 Section 870.4330 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN... Cardiopulmonary bypass on-line blood gas monitor. (a) Identification. A cardiopulmonary bypass on-line blood...

  10. 21 CFR 870.4330 - Cardiopulmonary bypass on-line blood gas monitor.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Cardiopulmonary bypass on-line blood gas monitor... Cardiopulmonary bypass on-line blood gas monitor. (a) Identification. A cardiopulmonary bypass on-line blood gas monitor is a device used in conjunction with a blood gas sensor to measure the level of gases in the...

  11. 21 CFR 870.4330 - Cardiopulmonary bypass on-line blood gas monitor.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Cardiopulmonary bypass on-line blood gas monitor... Cardiopulmonary bypass on-line blood gas monitor. (a) Identification. A cardiopulmonary bypass on-line blood gas monitor is a device used in conjunction with a blood gas sensor to measure the level of gases in the...

  12. 21 CFR 870.4330 - Cardiopulmonary bypass on-line blood gas monitor.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Cardiopulmonary bypass on-line blood gas monitor... Cardiopulmonary bypass on-line blood gas monitor. (a) Identification. A cardiopulmonary bypass on-line blood gas monitor is a device used in conjunction with a blood gas sensor to measure the level of gases in the...

  13. 21 CFR 870.4330 - Cardiopulmonary bypass on-line blood gas monitor.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Cardiopulmonary bypass on-line blood gas monitor... Cardiopulmonary bypass on-line blood gas monitor. (a) Identification. A cardiopulmonary bypass on-line blood gas monitor is a device used in conjunction with a blood gas sensor to measure the level of gases in the...

  14. On Line Instruction: An Opportunity to Re-Examine and Re-Invent Pedagogy

    ERIC Educational Resources Information Center

    Rosenthal, Irene

    2011-01-01

    One of the reasons the author agreed to teach a hybrid, on-line course last summer was specifically to either challenge or confirm her negative perceptions about on-line instruction. In order to continue to be an outspoken critic whenever administrators encouraged developing on-line courses for what she assumed were pecuniary considerations, she…

  15. 77 FR 55811 - Manufacturing Extension Partnership Advisory Board On-line Open Meeting

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-09-11

    ... National Institute of Standards and Technology Manufacturing Extension Partnership Advisory Board On-line... Manufacturing Extension Partnership (MEP) Advisory Board will hold an open, on-line meeting via webcast on... their remote location. Questions regarding the on-line meeting should be sent to the...

  16. On-Line Tutoring for Math Achievement Testing: A Controlled Evaluation

    ERIC Educational Resources Information Center

    Beal, Carole R.; Walles, Rena; Arroyo, Ivon; Woolf, Beverly P.

    2007-01-01

    We report the results of a controlled evaluation of an interactive on-line tutoring system for high school math achievement test problem solving. High school students (N = 202) completed a math pre-test and were then assigned by teachers to receive interactive on-line multimedia tutoring or their regular classroom instruction. The on-line tutored…

  17. On-line coupling of solid-phase extraction to gas chromatography-mass spectrometry to determine musk fragrances in wastewater.

    PubMed

    Vallecillos, Laura; Borrull, Francesc; Pocurull, Eva

    2014-10-17

    An on-line coupling solid-phase extraction (SPE) has been developed for the first time to preconcentrate trace amounts of 17 musk fragrances extensively used in personal care products (6 polycyclic musks, 3 nitro musks, 7 macrocyclic musks and 1 polycyclic musk degradation product) from wastewater samples, prior to analysis by gas chromatography and mass spectrometry through an on-column interface. A 10 mm × 2 mm I.D. precolumn packed with Oasis HLB (60 μm) or C18 (60 μm) was compared for the optimization of the solid-phase extraction process. The parameters affecting the transfer of the analytes from the precolumn to the GC system (e.g. flow-rate, temperature and solvent vapor exit time) as well as SPE parameters (e.g. sample flow, sample volume, elution solvent, etc.) were optimized. An organic modifier such as methanol was added to the sample before the extraction process to avoid adsorption problems. The use of the MS detector under selected ion monitoring acquisition enabled the analytes to be quantified at low ng L(-1) levels, preconcentrating only 10 mL of sample, and the limits of detection were between 1 and 30 ng L(-1). The method was applied for the determination of musk fragrances in wastewater samples from three urban wastewater treatment plants (WWTPs). The analysis of influent urban wastewater revealed that galaxolide, tonalide and ambrettolide were the most abundant musk compounds with concentrations ranging between 18 ng L(-1) and 45,091 ng L(-1), 852 ng L(-1) and 49,904 ng L(-1) and 507 ng L(-1) and 21,528 ng L(-1) respectively. The remaining musks were present at lower concentrations and two of the macrocyclic musk studied (musk MC4 and civetone) were not detected. The analysis of effluent wastewater showed a decrease in the concentrations of all of the compounds present in influent samples, with the decrease being more significantly in the case of polycyclic and nitro musks than for macrocyclic musks. Only HHCB-lactone remained constant or

  18. Ultratrace determination of cadmium by cold vapor atomic absorption spectrometry after preconcentration with a simplified cloud point extraction methodology.

    PubMed

    Manzoori, Jamshid L; Abdolmohammad-Zadeh, Hossein; Amjadi, Mohammad

    2007-02-15

    A simplified micelle-mediated extraction methodology for the preconcentration of ultratrace levels of cadmium as a prior step to its determination by cold vapor atomic absorption spectrometry (CV-AAS) has been developed. The methodology is based on the cloud point extraction (CPE) of cadmium at pH 8 by using the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5) without adding any chelating agent. Cadmium cold vapor was generated from 2ml of the extracted surfactant-rich phase by means of sodium tetrahydroborate (3%, w/v) as a reducing agent and hydrochloric acid (0.2mol l(-1)) as a carrier solution. Several important variables that affect the cloud point extraction and cold vapor cadmium generation efficiency were investigated and optimized. The preconcentration of only 50ml of solution in the presence of 0.06% (v/v) PONPE 7.5 gives an enhancement factor of 62. The calibration graph using the preconcentration system was linear in the range of 4-100ng l(-1) with a correlation coefficient of 0.9992. Detection limit (3s) obtained in the optimal conditions was 0.56ng l(-1). The relative standard deviation (R.S.D.) for six replicate determinations at 20ng l(-1) Cd level was 3.2%. The proposed method was successfully applied to the ultratrace determination of cadmium in water samples.

  19. Medium chain triglyceride (MCT) rich, paclitaxel loaded self nanoemulsifying preconcentrate (PSNP): a safe and efficacious alternative to Taxol.

    PubMed

    Patel, Ketan; Patil, Anand; Mehta, Miten; Gota, Vikram; Vavia, Pradeep

    2013-12-01

    The current work was aimed to develop Medium Chain Triglyceride (MCT) rich self nanoemulsifying preconcentrate of paclitaxel (PTX) for parenteral delivery. Very high concentrations of Cremophor EL and ethanol in Taxol have rendered patients to severe side effects. Years of extensive research on development of cost effective and safer vehicle for PTX, have failed to provide a promising replacement for Taxol. MCT was selected as oil owing to its parenteral acceptability, high solubilization capacity and multiple therapeutic benefits in cancer cachexia. PTX precipitation kinetics and reported toxicity profile of Kolliphor HS15 has favored its selection for PTX Self Nanoemulsifying Preconcentrate (PSNP). Presence of 30% free PEG in Kolliphor HS15 (PEG-15-hydroxystearate) restricts its miscibility with MCT, imposing significant challenge in development of MCT rich self nanoemulsifying preconcentrate. Removal of PEG layer from oil-surfactant mixture facilitated the formulation of PSNP with 51% w/w MCT. PSNP exhibited better precipitation kinetic profile, higher PTX loading with negligible hemolysis and histamine release compared to Taxol. PSNP was bioequivalent to Taxol, though V(d) and MRT was significantly higher than Taxol. PSNP showed distinctly better profile in inhibiting tumor growth and maintaining body weight with significantly higher % survival. Thus, PSNP can be a safer vehicle with potential clinical benefits.

  20. Dispersive liquid-liquid microextraction combined with online preconcentration MEKC for the determination of some phenoxyacetic acids in drinking water.

    PubMed

    Zhang, Yaohai; Jiao, Bining

    2013-09-01

    A fast and simple technique composed of dispersive liquid-liquid microextraction (DLLME) and online preconcentration MEKC with diode array detection was developed for the determination of four phenoxyacetic acids, 2,4,5-trichlorophenoxyacetic acid, 2,4-dichlorophenoxyacetic acid, 2,6-dichlorophenoxyacetic acid, and 4-chlorophenoxyacetic acid, in drinking water. The four phenoxyacetic acids were separated in reversed-migration MEKC to the baseline. About 145-fold increases in detection sensitivity were observed with online concentration strategy, compared with standard hydrodynamic injection (5 s at 25 mbar pressure). LODs ranged from 0.002 to 0.005 mg/L using only the online preconcentration procedures without any offline concentration of the extract. A DLLME procedure was used in combination with the proposed online preconcentration strategies, which achieved the determination of analytes at limits of quantification ranging from 0.2 to 0.5 μg/kg, which is far lower than the maximum residue limits established by China. The satisfactory recoveries obtained by DLMME spiked at two levels ranged from 67.2 to 99.4% with RSD <15%, making this proposed method suitable for the determination of phenoxyacetic acids in water samples.

  1. Spectrophotometric determination of trace aluminium content in parenteral solutions by combined cloud point preconcentration-flow injection analysis.

    PubMed

    Sombra, L; Luconi, M; Silva, M F; Olsina, R A; Fernandez, L

    2001-07-01

    A cloud point preconcentration and flow injection (FI) analysis methodology for aluminium(III) determination has been developed. The analyte in the initial aqueous solution was complexed with Chrome Azurol S (CAS) in the presence of the cationic surfactant benzyldimethyltetradecylammonium chloride (BDTAC). The absorption spectroscopic characteristics of the ternary complex [Al(III)-CAS-BDTAC] were examined in detail. The preconcentration step was carried out by means of the non-ionic surfactant polyethylene glycol p-nonylphenyl ether (PONPE 7.5). The enriched analyte solution was injected into an FI system using an HPLC pump. The chemical variables affecting the analytical performance of the combined methodology were studied and optimised. The developed approach was successfully applied to the determination of trace amounts of aluminium in parenteral solutions without previous treatment. Under the optimum experimental conditions, 99.9% extraction was achieved for a preconcentration factor of 50. The limit of detection was 1.12 x 10(-7) mol(-1). The calibration plot was linear over at least two orders of magnitude of aluminium concentration. The developed coupled methodology, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate for monitoring the aluminium concentration in parenteral nutrition.

  2. Paper-based analytical device for sampling, on-site preconcentration and detection of ppb lead in water.

    PubMed

    Satarpai, Thiphol; Shiowatana, Juwadee; Siripinyanond, Atitaya

    2016-07-01

    A simple and cost effectiveness procedure based on a paper based analytical device (PAD) for sampling, on-site preconcentration and determination of Pb(II) in water samples was developed. The inkjet printing method was used for patterning of PAD. Colorimetric assay was developed on a PAD for Pb(II) detection in µgL(-1) level. This µgL(-1) level detection limit was achieved by in situ- and on-site preconcentration of Pb(II) onto adsorption filter paper disc with a home-made holder before color development. Water sample was loaded onto a circular filter paper coated with zirconium silicate in 3% sodium carboxymethylcellulose for Pb(II) preconcentration. Subsequently, sodium rhodizonate in tartrate buffer solution (pH 2.8) was used as colorimetric reagent for direct Pb(II) detection on a PAD. Detection was achieved by measuring the pink color and recorded by scanner or digital camera. ImageJ software was used for measuring grey scale values. The calibration curve was linear in the range of 10µgL(-1) and 100µgL(-1), with a detection limit of 10µgL(-1). The developed method was successfully applied to the determination of Pb(II) in drinking water, tap water and surface water near electronic waste storage and the results were compared with those by graphite furnace atomic absorption spectroscopy (GF-AAS) with good agreement. PMID:27154707

  3. Application of modified simplex on the development of a preconcentration system for cadmium determination in sediments, food and cigarettes.

    PubMed

    Santos, Queila O; Moreno, Islania; Santos, Leandro Dos; Santos, Aldenor G; Souza, Valdinei S; Bezerra, Marcos A

    2016-05-13

    A modified simplex algorithm was used to optimize a system of preconcentration for cadmium determination in samples of sediments, cigarettes and food using flame atomic absorption spectrometry. The preconcentration system is based on the sorption of cadmium in a minicolumn packed with Amberlite XAD-2 resin functionalized with 3,4-dihydroxybenzoic acid (DHB). The optimized variables were pH and sampling flow rate and the optimum conditions found for these variables were, respectively 8.7 and 8.8 mL min-1. The developed system showed a preconcentration factor of 15.3, detection limit of 0.49 µg L-1, quantification limit of 1.65 µg L-1 and precision expressed as relative standard deviation (% RSD, n=10) of 5.9. The accuracy of the method was checked by analysis of estuary sediment certified reference material (NIST 1646-1). The cadmium concentrations found in sediment samples ranged from 1.73 and 1.90 µg g-1. In cigarette samples the results were 0.085 and 0.193 µg g-1, and in food samples (coriander and lettuce) the concentrations found of this metal were, respectively, 0.33 and 0.12 µg g-1. PMID:27192197

  4. Use of cloud-point preconcentration for spectrophotometric determination of trace amounts of antimony in biological and environmental samples.

    PubMed

    El-Sharjawy, Abdel-Azeem M; Amin, Alaa S

    2016-01-01

    This work presents a cloud-point extraction process using the micelle-mediated extraction method for simultaneous preconcentration and determination of Sb(III) and Sb(V) species in biological and environmental samples as a prior preconcentration step to their spectrophotometric determination. The analytical system is based on the selective reaction between Sb(III) and 3-dichloro-6-(3-carboxy-2-hydroxy-1-naphthylazo)quinoxaline (DCHNAQ) in the presence of cetyltrimethylammonium bromide (CTAB) and potassium iodide at pH 4.5. Total Sb concentration was determined after reduction of Sb(V) to Sb(III) in the presence of potassium iodide and ascorbic acid. The optimal reaction conditions and extraction were studied, and the analytical characteristics of the method (e.g., limits of detection and quantification, linear range, preconcentration, improvement factors) were obtained. Linearity for Sb(III) was obeyed in the range of 0.2-20 ng ml(-1). The detection and quantification limits for the determination of Sb(III) were 0.055 and 0.185 ng ml(-1), respectively. The method has a lower detection limit and wider linear range, inexpensive instrument, and low cost, and is more sensitive compared with most other methods. The interference effect of some anions and cations was also studied. The method was applied to the determination of Sb(III) in the presence of Sb(V) and total antimony in blood plasma, urine, biological, and water samples.

  5. Paper-based analytical device for sampling, on-site preconcentration and detection of ppb lead in water.

    PubMed

    Satarpai, Thiphol; Shiowatana, Juwadee; Siripinyanond, Atitaya

    2016-07-01

    A simple and cost effectiveness procedure based on a paper based analytical device (PAD) for sampling, on-site preconcentration and determination of Pb(II) in water samples was developed. The inkjet printing method was used for patterning of PAD. Colorimetric assay was developed on a PAD for Pb(II) detection in µgL(-1) level. This µgL(-1) level detection limit was achieved by in situ- and on-site preconcentration of Pb(II) onto adsorption filter paper disc with a home-made holder before color development. Water sample was loaded onto a circular filter paper coated with zirconium silicate in 3% sodium carboxymethylcellulose for Pb(II) preconcentration. Subsequently, sodium rhodizonate in tartrate buffer solution (pH 2.8) was used as colorimetric reagent for direct Pb(II) detection on a PAD. Detection was achieved by measuring the pink color and recorded by scanner or digital camera. ImageJ software was used for measuring grey scale values. The calibration curve was linear in the range of 10µgL(-1) and 100µgL(-1), with a detection limit of 10µgL(-1). The developed method was successfully applied to the determination of Pb(II) in drinking water, tap water and surface water near electronic waste storage and the results were compared with those by graphite furnace atomic absorption spectroscopy (GF-AAS) with good agreement.

  6. The effect of family therapy on the changes in the severity of on-line game play and brain activity in adolescents with on-line game addiction

    PubMed Central

    Han, Doug Hyun; Kim, Sun Mi; Lee, Young Sik; Renshaw, Perry F.

    2015-01-01

    We evaluated whether a brief 3-week family therapy intervention would change patterns of brain activation in response to affection and gaming cues in adolescents from dysfunctional families who met criteria for on-line game addiction. Fifteen adolescents with on-line game addiction and fifteen adolescents without problematic on-line game play and an intact family structure were recruited. Over 3 weeks, families were asked to carry out homework assignments focused on increasing family cohesion for more than 1 hour/day and 4 days/week. Before therapy, adolescents with on-line game addiction demonstrated decreased activity as measured by functional magnetic resonance imaging (fMRI) within the caudate, middle temporal gyrus, and occipital lobe in response to images depicting parental affection and increased activity of the middle frontal and inferior parietal in response scenes from on-line games, relative to healthy comparison subjects. Improvement in perceived family cohesion following 3 weeks of treatment was associated with an increase in the activity of the caudate nucleus in response to affection stimuli and was inversely correlated with changes in on-line game playing time. With evidence of brain activation changes in response to on-line game playing cues and images depicting parental love, the present findings suggest that family cohesion may be an important factor in the treatment of problematic on-line game playing. PMID:22698763

  7. The effect of family therapy on the changes in the severity of on-line game play and brain activity in adolescents with on-line game addiction.

    PubMed

    Han, Doug Hyun; Kim, Sun Mi; Lee, Young Sik; Renshaw, Perry F

    2012-05-31

    We evaluated whether a brief 3-week family therapy intervention would change patterns of brain activation in response to affection and gaming cues in adolescents from dysfunctional families who met criteria for on-line game addiction. Fifteen adolescents with on-line game addiction and fifteen adolescents without problematic on-line game play and an intact family structure were recruited. Over 3 weeks, families were asked to carry out homework assignments focused on increasing family cohesion for more than 1 hour/day and 4 days/week. Before therapy, adolescents with on-line game addiction demonstrated decreased activity as measured by functional magnetic resonance imaging (fMRI) within the caudate, middle temporal gyrus, and occipital lobe in response to images depicting parental affection and increased activity of the middle frontal and inferior parietal in response scenes from on-line games, relative to healthy comparison subjects. Improvement in perceived family cohesion following 3 weeks of treatment was associated with an increase in the activity of the caudate nucleus in response to affection stimuli and was inversely correlated with changes in on-line game playing time. With evidence of brain activation changes in response to on-line game playing cues and images depicting parental love, the present findings suggest that family cohesion may be an important factor in the treatment of problematic on-line game playing.

  8. On-line DNA analysis system with rapid thermal cycling

    DOEpatents

    Swerdlow, H.P.; Wittwer, C.T.

    1999-08-10

    This application describes an apparatus particularly suited for subjecting biological samples to any necessary sample preparation tasks, subjecting the sample to rapid thermal cycling, and then subjecting the sample to subsequent on-line analysis using one or more of a number of analytical techniques. The apparatus includes a chromatography device including an injection means, a chromatography pump, and a chromatography column. In addition, the apparatus also contains a capillary electrophoresis device consisting of a capillary electrophoresis column with an inlet and outlet end, a means of injection, and means of applying a high voltage to cause the differential migration of species of interest through the capillary column. Effluent from the liquid chromatography column passes over the inlet end of the capillary electrophoresis column through a tee structure and when the loading of the capillary electrophoresis column is desired, a voltage supply is activated at a precise voltage and polarity over a specific duration to cause sample species to be diverted from the flowing stream to the capillary electrophoresis column. A laser induced fluorescence detector preferably is used to analyze the products separated while in the electrophoresis column. 6 figs.

  9. On-line DNA analysis system with rapid thermal cycling

    DOEpatents

    Swerdlow, Harold P.; Wittwer, Carl T.

    1999-01-01

    An apparatus particularly suited for subjecting biological samples to any necessary sample preparation tasks, subjecting the sample to rapid thermal cycling, and then subjecting the sample to subsequent on-line analysis using one or more of a number of analytical techniques. The apparatus includes a chromatography device including an injection means, a chromatography pump, and a chromatography column. In addition, the apparatus also contains a capillary electrophoresis device consisting of a capillary electrophoresis column with an inlet and outlet end, a means of injection, and means of applying a high voltage to cause the differential migration of species of interest through the capillary column. Effluent from the liquid chromatography column passes over the inlet end of the capillary electrophoresis column through a tee structure and when the loading of the capillary electrophoresis column is desired, a voltage supply is activated at a precise voltage and polarity over a specific duration to cause sample species to be diverted from the flowing stream to the capillary electrophoresis column. A laser induced fluorescence detector preferably is used to analyze the products separated while in the electrophoresis column.

  10. On-line evidence for elaborative logical inferences in text.

    PubMed

    Lea, R B

    1995-11-01

    A model of propositional-logic reasoning proposed by M. D. S. Braine, B. J. Reiser, and B. Rumain (1984) claims that inferences such as "p or q; not p/therefore q" are made spontaneously by readers at the moment both premises are available. This claim is inconsistent with some evidence in the text-processing literature that suggests that only those inferences necessary for textual coherence are made spontaneously. In the present study, participants read stories in which a logical inference was not necessary to maintain textual coherence, and inference making was assessed with on-line probes. Two experiments tested logical forms central to Braine et al.'s model, and both indicated that participants were making the logical inferences. Two further experiments replicated this result with stories that did not begin with thematic titles. These findings support Braine et al.'s prediction that some propositional-logic inferences are made routinely in texts that do not require them for coherence. PMID:7490577

  11. Enterprise utilization of "always on-line" diagnostic study archive.

    PubMed

    McEnery, Kevin W; Suitor, Charles T; Thompson, Stephen K; Shepard, Jeffrey S; Murphy, William A

    2002-01-01

    To meet demands for enterprise image distribution, an "always on-line" image storage archive architecture was implemented before soft copy interpretation. It was presumed that instant availability of historical diagnostic studies would elicit a substantial utilization. Beginning November 1, 2000 an enterprise distribution archive was activated (Stentor, SanFrancisco, CA). As of August 8, 2001, 83,052 studies were available for immediate access without the need for retrieval from long-term archive. Image storage and retrieval logs for the period from June 12, 2001 to August 8, 2001 were analyzed. A total of 41,337 retrieval requests were noted for the 83,052 studies available as August 8, 2001. Computed radiography represented 16.8% of retrieval requests; digital radiography, 16.9%; computed tomography (CT), 44.5%; magnetic resonance (MR), 19.2%; and ultrasonography, 2.6%. A total of 51.5% of study retrievals were for studies less than 72 hours old. Study requests for cases greater than 100 days old represented 9.9% of all accessions, 9.7% of CT accessions, and 15.4% of MR accessions. Utilization of the archive indicates a substantial proportion of study retrievals for studies less than 72 hours after study completion. However, significant interest in historical CT and MR examinations was shown. PMID:12105703

  12. Haar wavelet processor for adaptive on-line image compression

    NASA Astrophysics Data System (ADS)

    Diaz, F. Javier; Buron, Angel M.; Solana, Jose M.

    2005-06-01

    An image coding processing scheme based on a variant of the Haar Wavelet Transform that uses only addition and subtraction is presented. After computing the transform, the selection and coding of the coefficients is performed using a methodology optimized to attain the lowest hardware implementation complexity. Coefficients are sorted in groups according to the number of pixels used in their computing. The idea behind it is to use a different threshold for each group of coefficients; these thresholds are obtained recurrently from an initial one. Parameter values used to achieve the desired compression level are established "on-line", adapting their values to each image, which leads to an improvement in the quality obtained for a preset compression level. Despite its adaptive characteristic, the coding scheme presented leads to a hardware implementation of markedly low circuit complexity. The compression reached for images of 512x512 pixels (256 grey levels) is over 22:1 (~0.4 bits/pixel) with a rmse of 8-10%. An image processor (excluding memory) prototype designed to compute the proposed transform has been implemented using FPGA chips. The processor for images of 256x256 pixels has been implemented using only one general-purpose low-cost FPGA chip, thus proving the design reliability and its relative simplicity.

  13. Development of on-line laser power monitoring system

    NASA Astrophysics Data System (ADS)

    Ding, Chien-Fang; Lee, Meng-Shiou; Li, Kuan-Ming

    2016-03-01

    Since the laser was invented, laser has been applied in many fields such as material processing, communication, measurement, biomedical engineering, defense industries and etc. Laser power is an important parameter in laser material processing, i.e. laser cutting, and laser drilling. However, the laser power is easily affected by the environment temperature, we tend to monitor the laser power status, ensuring there is an effective material processing. Besides, the response time of current laser power meters is too long, they cannot measure laser power accurately in a short time. To be more precisely, we can know the status of laser power and help us to achieve an effective material processing at the same time. To monitor the laser power, this study utilize a CMOS (Complementary metal-oxide-semiconductor) camera to develop an on-line laser power monitoring system. The CMOS camera captures images of incident laser beam after it is split and attenuated by beam splitter and neutral density filter. By comparing the average brightness of the beam spots and measurement results from laser power meter, laser power can be estimated. Under continuous measuring mode, the average measuring error is about 3%, and the response time is at least 3.6 second shorter than thermopile power meters; under trigger measuring mode which enables the CMOS camera to synchronize with intermittent laser output, the average measuring error is less than 3%, and the shortest response time is 20 millisecond.

  14. On-line phase measuring profilometry for a rotating object

    NASA Astrophysics Data System (ADS)

    Wang, Peng; Cao, Yiping; Yang, Xin; Peng, Kuang

    2014-11-01

    On-line phase measuring profilometry (OPMP) for a rotating object is proposed. N frames of circular sinusoidal grating patterns are designed in advance, in which the transmittance along the radial direction is sinusoidal and there is a fixed shifting phase pitch of 2π/N between every adjacent two grating patterns along the radial direction. While the measured object is rotating, the designed grating patterns are projected onto the rotating object by digital light processing and the corresponding deformed patterns caused by the object at different positions are captured by a charge coupled device camera. By pixel matching and rotation transformation with special marks, N frames of the deformed patterns of the object at the same position can be extracted. Hence, the rotating object can be reconstructed by the extracted deformed patterns. The results of computer emulation and experiment show the feasibility and validity of the proposed OPMP. Either the maximum measurement absolute error is 0.118 mm or the maximum root mean square error is 0.077 mm in the measured region of 0 to 25 mm.

  15. On-line monitoring of methane in sewer air

    PubMed Central

    Liu, Yiwen; Sharma, Keshab R.; Murthy, Sudhir; Johnson, Ian; Evans, Ted; Yuan, Zhiguo

    2014-01-01

    Methane is a highly potent greenhouse gas and contributes significantly to climate change. Recent studies have shown significant methane production in sewers. The studies conducted so far have relied on manual sampling followed by off-line laboratory-based chromatography analysis. These methods are labor-intensive when measuring methane emissions from a large number of sewers, and do not capture the dynamic variations in methane production. In this study, we investigated the suitability of infrared spectroscopy-based on-line methane sensors for measuring methane in humid and condensing sewer air. Two such sensors were comprehensively tested in the laboratory. Both sensors displayed high linearity (R2 > 0.999), with a detection limit of 0.023% and 0.110% by volume, respectively. Both sensors were robust against ambient temperature variations in the range of 5 to 35°C. While one sensor was robust against humidity variations, the other was found to be significantly affected by humidity. However, the problem was solved by equipping the sensor with a heating unit to increase the sensor surface temperature to 35°C. Field studies at three sites confirmed the performance and accuracy of the sensors when applied to actual sewer conditions, and revealed substantial and highly dynamic methane concentrations in sewer air. PMID:25319343

  16. Gated Treatment Delivery Verification With On-Line Megavoltage Fluoroscopy

    SciTech Connect

    Tai An; Christensen, James D.; Gore, Elizabeth; Khamene, Ali; Boettger, Thomas; Li, X. Allen

    2010-04-15

    Purpose: To develop and clinically demonstrate the use of on-line real-time megavoltage (MV) fluoroscopy for gated treatment delivery verification. Methods and Materials: Megavoltage fluoroscopy (MVF) image sequences were acquired using a flat panel equipped for MV cone-beam CT in synchrony with the respiratory signal obtained from the Anzai gating device. The MVF images can be obtained immediately before or during gated treatment delivery. A prototype software tool (named RTReg4D) was developed to register MVF images with phase-sequenced digitally reconstructed radiograph images generated from the treatment planning system based on four-dimensional CT. The image registration can be used to reposition the patient before or during treatment delivery. To demonstrate the reliability and clinical usefulness, the system was first tested using a thoracic phantom and then prospectively in actual patient treatments under an institutional review board-approved protocol. Results: The quality of the MVF images for lung tumors is adequate for image registration with phase-sequenced digitally reconstructed radiographs. The MVF was found to be useful for monitoring inter- and intrafractional variations of tumor positions. With the planning target volume contour displayed on the MVF images, the system can verify whether the moving target stays within the planning target volume margin during gated delivery. Conclusions: The use of MVF images was found to be clinically effective in detecting discrepancies in tumor location before and during respiration-gated treatment delivery. The tools and process developed can be useful for gated treatment delivery verification.

  17. Self-checking on-line testable static RAM

    NASA Technical Reports Server (NTRS)

    Chau, Savio N. (Inventor); Rennels, David A. (Inventor)

    1993-01-01

    This is a fault-tolerant random access memory for use in fault-tolerant computers. It comprises a plurality of memory chips each comprising a plurality of on-line testable and correctable memory cells disposed in rows and columns for holding individually addressable binary bits and provision for error detection incorporated into each memory cell for outputting an error signal whenever a transient error occurs therein. In one embodiment, each of the memory cells comprises a pair of static memory sub-cells for simultaneously receiving and holding a common binary data bit written to the memory cell and the error detection provision comprises comparator logic for continuously sensing and comparing the contents of the memory sub-cells to one another and for outputting the error signal whenever the contents do not match. In another embodiment, each of the memory cells comprises a static memory sub-cell and a dynamic memory sub-cell for simultaneously receiving and holding a common binary data bit written to the memory cell and the error detection provision comprises comparator logic for continuously sensing and comparing the contents of the static memory sub-cell to the dynamic memory sub-cell and for outputting the error signal whenever the contents do not match. Capability for correction of errors is also included.

  18. Evaluation of on-line DEMs for flood inundation modeling

    NASA Astrophysics Data System (ADS)

    Sanders, Brett F.

    2007-08-01

    Recent and highly accurate topographic data should be used for flood inundation modeling, but this is not always feasible given time and budget constraints so the utility of several on-line digital elevation models (DEMs) is examined with a set of steady and unsteady test problems. DEMs are used to parameterize a 2D hydrodynamic flood simulation algorithm and predictions are compared with published flood maps and observed flood conditions. DEMs based on airborne light detection and ranging (LiDAR) are preferred because of horizontal resolution, vertical accuracy (˜0.1 m) and the ability to separate bare-earth from built structures and vegetation. DEMs based on airborne interferometric synthetic aperture radar (IfSAR) have good horizontal resolution but gridded elevations reflect built structures and vegetation and therefore further processing may be required to permit flood modeling. IfSAR and shuttle radar topography mission (SRTM) DEMs suffer from radar speckle, or noise, so flood plains may appear with non-physical relief and predicted flood zones may include non-physical pools. DEMs based on national elevation data (NED) are remarkably smooth in comparison to IfSAR and SRTM but using NED, flood predictions overestimate flood extent in comparison to all other DEMs including LiDAR, the most accurate. This study highlights utility in SRTM as a global source of terrain data for flood modeling.

  19. Virtual laboratories: Collaborative environments and facilities-on-line

    SciTech Connect

    Thomas, C.E. Jr.; Cavallini, J.S.; Seweryniak, G.R.; Kitchens, T.A.; Hitchcock, D.A.; Scott, M.A.; Welch, L.C.; Aiken, R.J. |; Stevens, R.L.

    1995-07-01

    The Department of Energy (DOE) has major research laboratories in a number of locations in the US, typically co-located with large research instruments or research facilities valued at tens of millions to even billions of dollars. Present budget exigencies facing the entire nation are felt very deeply at DOE, just as elsewhere. Advances over the last few years in networking and computing technologies make virtual collaborative environments and conduct of experiments over the internetwork structure a possibility. The authors believe that development of these collaborative environments and facilities-on-line could lead to a ``virtual laboratory`` with tremendous potential for decreasing the costs of research and increasing the productivity of their capital investment in research facilities. The majority of these cost savings would be due to increased productivity of their research efforts, better utilization of resources and facilities, and avoiding duplication of expensive facilities. A vision of how this might all fit together and a discussion of the infrastructure necessary to enable these developments is presented.

  20. Using on-line altered auditory feedback treating Parkinsonian speech

    NASA Astrophysics Data System (ADS)

    Wang, Emily; Verhagen, Leo; de Vries, Meinou H.

    2005-09-01

    Patients with advanced Parkinson's disease tend to have dysarthric speech that is hesitant, accelerated, and repetitive, and that is often resistant to behavior speech therapy. In this pilot study, the speech disturbances were treated using on-line altered feedbacks (AF) provided by SpeechEasy (SE), an in-the-ear device registered with the FDA for use in humans to treat chronic stuttering. Eight PD patients participated in the study. All had moderate to severe speech disturbances. In addition, two patients had moderate recurring stuttering at the onset of PD after long remission since adolescence, two had bilateral STN DBS, and two bilateral pallidal DBS. An effective combination of delayed auditory feedback and frequency-altered feedback was selected for each subject and provided via SE worn in one ear. All subjects produced speech samples (structured-monologue and reading) under three conditions: baseline, with SE without, and with feedbacks. The speech samples were randomly presented and rated for speech intelligibility goodness using UPDRS-III item 18 and the speaking rate. The results indicted that SpeechEasy is well tolerated and AF can improve speech intelligibility in spontaneous speech. Further investigational use of this device for treating speech disorders in PD is warranted [Work partially supported by Janus Dev. Group, Inc.].

  1. On-Line Loss of Control Detection Using Wavelets

    NASA Technical Reports Server (NTRS)

    Brenner, Martin J. (Technical Monitor); Thompson, Peter M.; Klyde, David H.; Bachelder, Edward N.; Rosenthal, Theodore J.

    2005-01-01

    Wavelet transforms are used for on-line detection of aircraft loss of control. Wavelet transforms are compared with Fourier transform methods and shown to more rapidly detect changes in the vehicle dynamics. This faster response is due to a time window that decreases in length as the frequency increases. New wavelets are defined that further decrease the detection time by skewing the shape of the envelope. The wavelets are used for power spectrum and transfer function estimation. Smoothing is used to tradeoff the variance of the estimate with detection time. Wavelets are also used as front-end to the eigensystem reconstruction algorithm. Stability metrics are estimated from the frequency response and models, and it is these metrics that are used for loss of control detection. A Matlab toolbox was developed for post-processing simulation and flight data using the wavelet analysis methods. A subset of these methods was implemented in real time and named the Loss of Control Analysis Tool Set or LOCATS. A manual control experiment was conducted using a hardware-in-the-loop simulator for a large transport aircraft, in which the real time performance of LOCATS was demonstrated. The next step is to use these wavelet analysis tools for flight test support.

  2. Building collaboration tools and access to on-line facilities

    SciTech Connect

    Agarwal, D.; Sachs, S.

    1996-11-01

    Network-based facilities will allow researchers at different locations to collaborate on experiments as if they all were together in the same laboratory. The expected value of these geographically distributed environments includes substantially increased effectiveness in doing science, and an enabling capability for analytical and high-value production use by industry. The Distributed, Collaboratory Experiment Environments (DCEE) Program consists of four projects that were established to build prototype remote experiment and collaborative environments. The work undertaken in this project represents some of the research and development of the mechanisms and infrastructure required to make collaboratories a reality. Some of these mechanisms have already been developed. Several other mechanisms, such as data dissemination, resource management for the sharing of experiment control, safety and security, electronic notebooks, elements of telepresence, and integrated user interfaces need further research and development. The pilot application for these collaborative tools is the Advanced Light Source (ALS) Beamline 7.0 at the Ernest Orlando Lawrence Berkeley Laboratory. The ALS is a particle accelerator and is a source of very high brilliance soft X-ray beams. One experimental facility is the Spectro-Microscopy Facility Beamline 7.0. Through this project, the Spectro-Microscopy Facility will be opened up to users from a wide range of organizations. The goal is to build software that will not only put the ALS Beamline 7.0 on-line, but will also serve as building blocks for future collaboratory development.

  3. EnviroNET: On-line information for LDEF

    NASA Technical Reports Server (NTRS)

    Lauriente, Michael

    1993-01-01

    EnviroNET is an on-line, free-form database intended to provide a centralized repository for a wide range of technical information on environmentally induced interactions of use to Space Shuttle customers and spacecraft designers. It provides a user-friendly, menu-driven format on networks that are connected globally and is available twenty-four hours a day - every day. The information, updated regularly, includes expository text, tabular numerical data, charts and graphs, and models. The system pools space data collected over the years by NASA, USAF, other government research facilities, industry, universities, and the European Space Agency. The models accept parameter input from the user, then calculate and display the derived values corresponding to that input. In addition to the archive, interactive graphics programs are also available on space debris, the neutral atmosphere, radiation, magnetic fields, and the ionosphere. A user-friendly, informative interface is standard for all the models and includes a pop-up help window with information on inputs, outputs, and caveats. The system will eventually simplify mission analysis with analytical tools and deliver solutions for computationally intense graphical applications to do 'What if...' scenarios. A proposed plan for developing a repository of information from the Long Duration Exposure Facility (LDEF) for a user group is presented.

  4. On-line monitoring of methane in sewer air

    NASA Astrophysics Data System (ADS)

    Liu, Yiwen; Sharma, Keshab R.; Murthy, Sudhir; Johnson, Ian; Evans, Ted; Yuan, Zhiguo

    2014-10-01

    Methane is a highly potent greenhouse gas and contributes significantly to climate change. Recent studies have shown significant methane production in sewers. The studies conducted so far have relied on manual sampling followed by off-line laboratory-based chromatography analysis. These methods are labor-intensive when measuring methane emissions from a large number of sewers, and do not capture the dynamic variations in methane production. In this study, we investigated the suitability of infrared spectroscopy-based on-line methane sensors for measuring methane in humid and condensing sewer air. Two such sensors were comprehensively tested in the laboratory. Both sensors displayed high linearity (R2 > 0.999), with a detection limit of 0.023% and 0.110% by volume, respectively. Both sensors were robust against ambient temperature variations in the range of 5 to 35°C. While one sensor was robust against humidity variations, the other was found to be significantly affected by humidity. However, the problem was solved by equipping the sensor with a heating unit to increase the sensor surface temperature to 35°C. Field studies at three sites confirmed the performance and accuracy of the sensors when applied to actual sewer conditions, and revealed substantial and highly dynamic methane concentrations in sewer air.

  5. On-line modeling tutorials for emergency managers

    SciTech Connect

    Newsom, D.E.

    1988-01-01

    The Federal Emergency Management Agency (FEMA) maintains two simulation models of interest to Federal, State, and local government managers: MESORAD, a model of radiological plume dispersion and dose; and IDYNEV, a model of traffic movement during evacuation. Users of these models include government staff and technical consultants with simulation experience ranging from extensive to none. To train these users, Argonne National Laboraory has developed two on-line tutorials. The tutorials provide a self-paced, interactive mode of learning about the models. Though user manuals about the models exist, the tutorials afford self-contained instruction to users who lack access to the manuals. The tutorials describe: dose assessment and transportation analysis using computer models; the input parameters needed by the models; how to use forms management software to prepare the data; and how to run the models and view outputs. The tutorials have evolved with upgrades to the models, including the need at various times to emulate three different forms management packages. The tutorials have been used for individual study; in continuing education courses at FEMA's Emergency Management Institute; and are being considered for college classroom use. Persons trained in using the models have applied them to actual emergency planning problems for nuclear power plants. 4 refs., 3 figs., 2 tabs.

  6. On-line range images registration with GPGPU

    NASA Astrophysics Data System (ADS)

    Będkowski, J.; Naruniec, J.

    2013-03-01

    This paper concerns implementation of algorithms in the two important aspects of modern 3D data processing: data registration and segmentation. Solution proposed for the first topic is based on the 3D space decomposition, while the latter on image processing and local neighbourhood search. Data processing is implemented by using NVIDIA compute unified device architecture (NIVIDIA CUDA) parallel computation. The result of the segmentation is a coloured map where different colours correspond to different objects, such as walls, floor and stairs. The research is related to the problem of collecting 3D data with a RGB-D camera mounted on a rotated head, to be used in mobile robot applications. Performance of the data registration algorithm is aimed for on-line processing. The iterative closest point (ICP) approach is chosen as a registration method. Computations are based on the parallel fast nearest neighbour search. This procedure decomposes 3D space into cubic buckets and, therefore, the time of the matching is deterministic. First technique of the data segmentation uses accele-rometers integrated with a RGB-D sensor to obtain rotation compensation and image processing method for defining pre-requisites of the known categories. The second technique uses the adapted nearest neighbour search procedure for obtaining normal vectors for each range point.

  7. A fully automated and fast method using direct sample injection combined with fused-core column on-line SPE-HPLC for determination of ochratoxin A and citrinin in lager beers.

    PubMed

    Lhotská, Ivona; Šatínský, Dalibor; Havlíková, Lucie; Solich, Petr

    2016-05-01

    A new fast and sensitive method based on on-line solid-phase extraction on a fused-core precolumn coupled to liquid chromatography with fluorescence detection has been developed for ochratoxin A (OTA) and citrinin (CIT) determination in lager beer samples. Direct injection of 100 μL filtered beer samples into an on-line SPE-HPLC system enabled fast and effective sample extraction including separation in less than 6 min. Preconcentration of OTA and CIT from beer samples was performed on an Ascentis Express RP C18 guard column (5 × 4.6 mm), particle size 2.7 μm, with a mobile phase of methanol/0.5% aqueous acetic acid pH 2.8 (30:70, v/v) at a flow rate of 2.0 mL min(-1). The flow switch from extraction column to analytical column in back-flush mode was set at 2.0 min and the separation was performed on the fused-core column Ascentis Express Phenyl-Hexyl (100 × 4.6 mm), particle size 2.7 μm, with a mobile phase acetonitrile/0.5% aqueous acetic acid pH 2.8 in a gradient elution at a flow rate of 1.0 mL min(-1) and temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 335/497 nm. The accuracy of the method, defined as the mean recoveries of OTA and CIT from light and dark beer samples, was in the range 98.3-102.1%. The method showed high sensitivity owing to on-line preconcentration; LOQ values were found to be 10 and 20 ng L(-1) for OTA and CIT, respectively. The found values of OTA and CIT in all tested light, dark and wheat beer samples were significantly below the maximum tolerable limits (3.0 μg kg(-1) for OTA and 2000 μg kg(-1) for CIT) set by the European Union. PMID:26993307

  8. Fully 3D-Printed Preconcentrator for Selective Extraction of Trace Elements in Seawater.

    PubMed

    Su, Cheng-Kuan; Peng, Pei-Jin; Sun, Yuh-Chang

    2015-07-01

    In this study, we used a stereolithographic 3D printing technique and polyacrylate polymers to manufacture a solid phase extraction preconcentrator for the selective extraction of trace elements and the removal of unwanted salt matrices, enabling accurate and rapid analyses of trace elements in seawater samples when combined with a quadrupole-based inductively coupled plasma mass spectrometer. To maximize the extraction efficiency, we evaluated the effect of filling the extraction channel with ordered cuboids to improve liquid mixing. Upon automation of the system and optimization of the method, the device allowed highly sensitive and interference-free determination of Mn, Ni, Zn, Cu, Cd, and Pb, with detection limits comparable with those of most conventional methods. The system's analytical reliability was further confirmed through analyses of reference materials and spike analyses of real seawater samples. This study suggests that 3D printing can be a powerful tool for building multilayer fluidic manipulation devices, simplifying the construction of complex experimental components, and facilitating the operation of sophisticated analytical procedures for most sample pretreatment applications.

  9. Production of 191Pt radiotracer with high specific activity for the development of preconcentration procedures

    NASA Astrophysics Data System (ADS)

    Parent, M.; Strijckmans, K.; Cornelis, R.; Dewaele, J.; Dams, R.

    1994-04-01

    A radiotracer of Pt with suitable nuclear characteristics and high specific activity (i.e. activity to mass ratio) is a powerful tool when developing preconcentration methods for the determination of base-line levels of Pt in e.g. environmental and biological samples. Two methods were developed for the production of 191Pt with high specific activity and radionuclidic purity: (1) via the 190Pt(n, γ) 191Pt reaction by neutron irradiation of enriched Pt in a nuclear reactor at high neutron fluence rate and (2) via the 191Ir(p, n) 191Pt reaction by proton irradiation of natural Ir with a cyclotron, at an experimentally optimized proton energy. For the latter method it was necessary to separate Pt from the Ir matrix. For that reason either liquid-liquid extraction with dithizone or adsorption chromatography were used. The yields, the specific activities and the radionuclidic purities were experimentally determined as a function of the proton energy and compared to the former method. The half-life of 191Pt was accurately determined to be 2.802 ± 0.025 d.

  10. Carminic acid modified anion exchanger for the removal and preconcentration of Mo(VI) from wastewater.

    PubMed

    El-Moselhy, Medhat Mohamed; Sengupta, Arup K; Smith, Ryan

    2011-01-15

    Removal and preconcentration of Mo(VI) from water and wastewater solutions was investigated using carminic acid modified anion exchanger (IRA743). Various factors influencing the adsorption of Mo(VI), e.g. pH, initial concentration, and coexisting oxyanions were studied. Adsorption reached equilibrium within <10 min and was independent of initial concentration of Mo(VI). Studies were performed at different pH values to find the pH at which maximum adsorption occurred and was determined to be at a pH between 4.0 and 6.0. The Langmuir adsorption capacity (q(max)) was found to be 13.5mg Mo(VI)/g of the adsorbent. The results showed that modification of IRA743 with carminic acid is suitable for the removal of Mo(VI), as molybdate, from water and wastewater samples. The concentration of Mo(VI) was determined spectrophotometrically using bromopyrogallol red as a complexation reagent. This allows the determination of Mo(VI) in the range 1.0-100.0 μg/mL. The obtained material was subjected to efficient regeneration. PMID:20943315

  11. Dissimilar viscosity induced sample pre-concentration in elecrokinetic nanofluidic channels

    NASA Astrophysics Data System (ADS)

    Wink, Dean; Shelton, Elijah; Pennathur, Sumita; Storey, Brian

    2013-11-01

    Nanofluidic analysis systems boast many advantages: portability, small sample handling, short processing times, and potential for integration with mobile electronics. However, such systems face the challenge of detecting increasingly small volumes of sample at low concentrations. In this work, we demonstrate a unique pre-concentration technique in electrokinetic nanofluidic systems based on a viscosity mismatch between two fluids. In nanofluidic electrokinetic systems, finite electric double layers (EDL) lead to non-uniform electric potentials and transverse concentration distributions. Therefore, when the EDL is comparable in size to the channel height, negatively charged ions are repelled from negatively charged walls and preferentially populate the channel centerline. Furthermore, an axial piecewise viscosity distribution induces internal pressure gradients within the channel. These force the ions to move at a different average velocities based on the pressure gradient being favorable or adverse, leading to focusing. To experimentally probe this phenomenon, we electrokinetically inject solutions of borate buffer with and without glycerol (to change the viscosity) and use a fluorescent tracer dye to visualize the flow. We perform the injections in cross-geometry channels of 20 micron, 1 micron, and 250 nanometer depths. We measure fluorescence at 5, 10 and 15 mm distances from junction. Enhancement is characterized by comparing intensities to control measurements for systems with uniform viscosity.

  12. Rapid Preconcentration for Liquid Chromatography-Mass Spectrometry Assay of Trace Level Neuropeptides

    NASA Astrophysics Data System (ADS)

    Zhou, Ying; Mabrouk, Omar S.; Kennedy, Robert T.

    2013-11-01

    Measurement of neuropeptides in the brain through in vivo microdialysis sampling provides direct correlation between neuropeptide concentration and brain function. Capillary liquid chromatography-multistage mass spectrometry (CLC-MSn) has proven to be effective at measuring endogenous neuropeptides in microdialysis samples. In the method, microliter samples are concentrated onto nanoliter volume packed beds before ionization and mass spectrometry analysis. The long times required for extensive preconcentration present a barrier to routine use because of the many samples that must be analyzed and instability of neuropeptides. In this study, we evaluated the capacity of 75 μm inner diameter (i.d.) capillary column packed with 10 μm reversed phase particles for increasing the throughput in CLC-MSn based neuropeptide measurement. Coupling a high injection flow rate for fast sample loading/desalting with a low elution flow rate to maintain detection sensitivity, this column has reduced analysis time from ˜30 min to 3.8 min for 5 μL sample, with 3 pM limit of detection (LOD) for enkephalins and 10 pM LOD for dynorphin A1-8 in 5 μL sample. The use of isotope-labeled internal standard lowered peptide signal variation to less than 5 %. This method was validated for in vivo detection of Leu and Met enkephalin with microdialysate collected from rat globus pallidus. The improvement in speed and stability makes CLC-MSn measurement of neuropeptides in vivo more practical.

  13. Factorial design in the optimization of preconcentration procedure for lead determination by FAAS.

    PubMed

    Soylak, Mustafa; Narin, Ibrahim; Bezerra, Marcos de Almeida; Ferreira, Sérgio Luís Costa

    2005-02-28

    The present paper proposes a preconcentration procedure for lead determination using flame atomic absorption spectrometry (FAAS). It is based on lead(II) ions extraction as brilliant cresyl blue (BCB) complex and its sorption onto Diaion HP-2MG, a methacrylic ester copolymer. The optimization step was carried out using factorial design and the variables studied were pH, shaking time and reagent concentration. In the established experimental conditions, lead can be determinate with a limit of detection of 3.7mugL(-1) lead (N = 20) and a relative standard deviation of 7% for a lead concentration of 100mugL(-1). The accuracy was confirmed by analysis of a certified reference material, the stream sediment furnished by National Research Centre for Certified Reference Materials (NRCCRM), China (GBW 07310). Effect of other ions in the procedure proposed was also studied. The method was applied for lead determination in real samples of water, tea, soil and dust. Tests of addition/recovery in the experiments for lead determination in water samples revealed that the proposed procedure could be applied satisfactorily for analysis of these samples. PMID:18969885

  14. Thermal modified Kaolinite as useful material for separation and preconcentration of trace amounts of manganese ions.

    PubMed

    Afzali, Darush; Taher, Mohammad Ali; Mostafavi, Ali; Mobarakeh, Sayed Ziae Mohammadi

    2005-01-30

    This work assesses for the first time the potential of natural Kaolinite as adsorptive material for preconcentration of metal traces. Manganese is quantitatively retained by 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) on thermal modified Kaolinite by column method in pH range of 8.5-10.0 at flow rate of 2mlmin(-1). Manganese was removed from column with 5.0ml of H(2)SO(4) 4moll(-1) and determined by flame atomic absorption spectrometric at 279.5nm. In this case, 0.lmug of manganese can be concentrated from 800ml of aqueous sample (where concentration is as low as 0.125mugl(-1)). Detection limit is 4.3mugl(-1) (3delta(bl)m(-1)) and analytical curve is linear in the 0.02-10mgl(-1) in final solution with correlation coefficient 0.9997 and relative standard deviation for eight replicate determination of 5mug of manganese in final solution is 0.71%. The interference of a large number of anions and cations has been studied in detail to optimize the conditions and method was successfully applied for determination of manganese in complex materials. PMID:18969822

  15. HF-LPME as a green alternative for the preconcentration of nickel in natural waters.

    PubMed

    Vergel, Cristina; Montoya, Rocío; Mendiguchía, Carolina; García-Vargas, Manuel; Moreno, Carlos

    2012-08-01

    In the last years, some analytical methodologies have been identified as a source of pollution, receiving increasing attention to decrease their impact on the environment. In this sense, the so-called solvent-less methodologies appear as a green alternative to reduce the volume of solvents used in many sample treatment procedures and, consequently, the volume of toxic wastes produced. Among these techniques, analytical methodologies based on liquid-phase microextraction are being continuously developed, although most applications are focused on organic compounds. In this work, a three-phase hollow-fibre liquid-phase microextraction (HF-LPME) system has been developed for the preconcentration of nickel in natural waters, prior to the analysis by atomic absorption spectrometry. Under optimum conditions, the new system allowed an enrichment factor of 29.80 to be obtained after 60 min of experiment, and it was successfully applied to the determination of nickel in both saline and non-saline water samples, at ppb and ppt levels. The results were compared with those obtained using a well-established methodology based on liquid solvent extraction showing no significant differences (α = 0.05) between both values. In addition, the new HF-LPME presents the advantages of a green analytical technique, as its greenness profile shows, with the additional reduction of sample manipulation and time cost. PMID:22402732

  16. Improved pre-concentration and detection methods for volatile sulphur breath constituents.

    PubMed

    Mochalski, Paweł; Wzorek, Beata; Sliwka, Ireneusz; Amann, Anton

    2009-07-01

    Suitability of different types of pre-concentration (solid phase microextraction and sorbent trapping) and detection (flame photometric detector (FPD) and mass selective detector (MSD)) for gas chromatographic determination of sulphur-containing compounds (H2S, MeSH, EtSH, DMS, COS and CS2) in breath-gas was assessed in this study. Several factors like influence of humidity, influence of oxygen, or stability of target compounds in extraction vessels (SPME vials and sorbent tubes) were investigated. Despite poor stability of VSCs in SPME vials and matrix effects (unfavorable influence of humidity), SPME was found to be a fast and reliable enrichment method, which coupled with mass selective detector provided satisfactory LODs of target compounds at the ppt level (from 0.15 ppb for CS2 to 2.3 ppb for H2S). Application of sorbent trapping with two-bed sorbent tubes containing Tenax TA and Carboxen 1000 gave excellent LODs (0.03-0.3 ppb for 200 ml sample and MSD). Stability of investigated VSCs in sorbents was found to be very poor (30-40% losses after 2 h). FPD showed satisfactory sensitivity only when it was coupled with sorbent trapping. Breath samples were collected into Tedlar bags in a CO2-controlled manner. Humidity was removed during sampling (permeation dryer--Nafion) to avoid unfavorable water dependent effects during analysis.

  17. Modeling the liquid filling in capillary well microplates for analyte preconcentration.

    PubMed

    Yu, Yang; Wang, Xuewei; Ng, Tuck Wah

    2012-06-15

    An attractive advantage of the capillary well microplate approach is the ability to conduct evaporative analyte preconcentration. We advance the use of hydrophobic materials for the wells which apart from reducing material loss through wetting also affords self entry into the well when the droplet size reduces below a critical value. Using Surface Evolver simulation without gravity, we find the critical diameters D(c) fitting very well with theoretical results. When simulating the critical diameters D(c)(G) with gravity included, the gravitational effect could only be ignored when the liquid volumes were small (difference of 5.7% with 5 μL of liquid), but not when the liquid volumes were large (differences of more than 22% with 50 μL of liquid). From this, we developed a modifying equation from a series of simulation results made to describe the gravitational effect. This modifying equation fitted the simulation results well in our simulation range (100°≤θ≤135° and 1 μL≤V≤200 μL). In simulating the condition of multiple wells underneath each droplet, we found that having more holes did not alter the critical diameters significantly. Consequently, the modifying relation should also generally express the critical diameter for multiple wells under a droplet.

  18. On-chip DNA preconcentration in different media conductivities by electrodeless dielectrophoresis

    PubMed Central

    Li, Shunbo; Ye, Ziran; Hui, Yu Sanna; Gao, Yibo; Jiang, Yusheng; Wen, Weijia

    2015-01-01

    Electrodeless dielectrophoresis is the best choice to achieve preconcentration of nanoparticles and biomolecules due to its simple, robust, and easy implementation. We designed a simple chip with microchannels and nano-slits in between and then studied the trapping of DNA in high conductive medium and low conductive medium, corresponding to positive and negative dielectrophoresis (DEP), respectively. It is very important to investigate the trapping in media with different conductivities since one always has to deal with the sample solutions with different conductivities. The trapping process was analyzed by the fluorescent intensity changes. The results showed that DNA could be trapped at the nano-slit in both high and low conductive media in a lower electric field strength (10 V/cm) compared to the existing methods. This is a significant improvement to suppress the Joule heating effect in DEP related experiments. Our work may give insight to researchers for DNA trapping by a simple and low cost device in the Lab-on-a-Chip system. PMID:26487901

  19. Fully 3D-Printed Preconcentrator for Selective Extraction of Trace Elements in Seawater.

    PubMed

    Su, Cheng-Kuan; Peng, Pei-Jin; Sun, Yuh-Chang

    2015-07-01

    In this study, we used a stereolithographic 3D printing technique and polyacrylate polymers to manufacture a solid phase extraction preconcentrator for the selective extraction of trace elements and the removal of unwanted salt matrices, enabling accurate and rapid analyses of trace elements in seawater samples when combined with a quadrupole-based inductively coupled plasma mass spectrometer. To maximize the extraction efficiency, we evaluated the effect of filling the extraction channel with ordered cuboids to improve liquid mixing. Upon automation of the system and optimization of the method, the device allowed highly sensitive and interference-free determination of Mn, Ni, Zn, Cu, Cd, and Pb, with detection limits comparable with those of most conventional methods. The system's analytical reliability was further confirmed through analyses of reference materials and spike analyses of real seawater samples. This study suggests that 3D printing can be a powerful tool for building multilayer fluidic manipulation devices, simplifying the construction of complex experimental components, and facilitating the operation of sophisticated analytical procedures for most sample pretreatment applications. PMID:26101898

  20. Electrokinetic protein preconcentration using a simple glass/poly(dimethylsiloxane) microfluidic chip.

    PubMed

    Kim, Sun Min; Burns, Mark A; Hasselbrink, Ernest F

    2006-07-15

    We discovered that a protein concentration device can be constructed using a simple one-layer fabrication process. Microfluidic half-channels are molded using standard procedures in PDMS; the PDMS layer is reversibly bonded to a glass base such as a microscope slide. The microfluidic channels are chevron-shaped, in mirror image orientation, with their apexes designed to pass within approximately 20 microm of each other, forming a thin-walled section between the channels. When an electric field is applied across this thin-walled section, negatively charged proteins are observed to concentrate on the anode side of it. About 10(3)-10(6)-fold protein concentration was achieved in 30 min. Subsequent separation of two different concentrated proteins is easily achieved by switching the direction of the electric field in the direction parallel to the thin-walled section. We hypothesize that a nanoscale channel forms between the PDMS and the glass due to the weak, reversible bonding method. This hypothesis is supported by the observation that, when the PDMS and glass are irreversibly bonded, this phenomenon is not observed until a very high E-field was applied and dielectric breakdown of the PDMS is observed. We therefore suspect that the ion exclusion-enrichment effect caused by electrical double layer overlapping induces cationic selectivity of this nanochannel. This simple on-chip protein preconcentration and separation device could be a useful component in practically any PDMS-on-glass microfluidic device used for protein assays.

  1. Nanofluidic preconcentration device in a straight microchannel using ion concentration polarization.

    PubMed

    Ko, Sung Hee; Song, Yong-Ak; Kim, Sung Jae; Kim, Myungji; Han, Jongyoon; Kang, Kwan Hyoung

    2012-11-01

    In this paper, we introduce a simple, straight microchannel design for a nanofluidic protein concentration device. Compared with concentration devices previously developed, the anode channel and cathode channel in this new concentration scheme are both integrated into a straight microchannel, with one inlet and one outlet. Most of the functions of a conventional two-channel concentration device can be achieved by this concentration device, and the efficiency of sample accumulation can be controlled by the dimension of the Nafion membrane. Also, the operating mechanism of this device was tested on various material combinations such as PDMS (polydimethyl-siloxane) channel-glass substrate and silicon channel-PDMS substrate. Using a combined PDMS-silicon device which was sealed reversibly without plasma bonding, surface based immunoassay for concentrator-enhanced detection of clinically relevant samples such as C-reactive protein (CRP) was demonstrated. As a result, it was possible to enhance the detection sensitivity of the immunoassay by more than 500 folds compared to the immunoassay without preconcentration process.

  2. On-chip DNA preconcentration in different media conductivities by electrodeless dielectrophoresis.

    PubMed

    Li, Shunbo; Ye, Ziran; Hui, Yu Sanna; Gao, Yibo; Jiang, Yusheng; Wen, Weijia

    2015-09-01

    Electrodeless dielectrophoresis is the best choice to achieve preconcentration of nanoparticles and biomolecules due to its simple, robust, and easy implementation. We designed a simple chip with microchannels and nano-slits in between and then studied the trapping of DNA in high conductive medium and low conductive medium, corresponding to positive and negative dielectrophoresis (DEP), respectively. It is very important to investigate the trapping in media with different conductivities since one always has to deal with the sample solutions with different conductivities. The trapping process was analyzed by the fluorescent intensity changes. The results showed that DNA could be trapped at the nano-slit in both high and low conductive media in a lower electric field strength (10 V/cm) compared to the existing methods. This is a significant improvement to suppress the Joule heating effect in DEP related experiments. Our work may give insight to researchers for DNA trapping by a simple and low cost device in the Lab-on-a-Chip system. PMID:26487901

  3. Determination of Trace Mercury by Cloud Point Extraction Preconcentration Coupled with Spectrophotometry

    NASA Astrophysics Data System (ADS)

    Sohrabi, Mahmoud Reza; Farokhi, Elham; Adnani, Atena; Ziaian, Mona

    A new micell-mediated phase separation method for preconcentration of ultra-trace quantities of mercury as a prior step to its determination spectrophotometry has been developed. The method is based on the Cloud Point Extraction (CPE) of mercury with Triton X-100 in the absence of chelating agent. Mercury react with sodium diethyldithiocarbamate (DDTC) in a surfactant solution yielding a hydrophobic complex, which then is entrapped in surfactant micelles. Separation of the two phases was accomplished by centrifugation for 10 min at 4000 rpm. Under the optimum conditions i.e., pH 9.0, cloud point temperature 45°C, [DDTC] = 1.6x10-5 mol L-1, [Triton X-114] = 0.032%. Analytical graphs were rectilinear in the concentration range of 4-240 µg L-1 and relative standard deviation for five replicate determinations of Mercury at 8 (μg L-1) concentration level, were 1.9%, respectively (n = 5, c = 8 µg L-1).

  4. Ion-exchange preconcentration and determination of vanadium in milk samples by electrothermal atomic absorption spectrometry.

    PubMed

    López-García, Ignacio; Viñas, Pilar; Romero-Romero, Rafael; Hernández-Córdoba, Manuel

    2009-06-15

    A new method for the electrothermal atomic absorption spectrometric determination of vanadium in milk and infant formulas using suspensions to avoid the need for previous dissolution of samples is described. Sensitivity is improved by a procedure based on preconcentration and removal of the matrix, using ion-exchange (Dowex 1X8-100). Suspensions of 15% (m/v) infant formula samples were prepared in a medium containing 0.05M sodium citrate (pH 7.2) and passed through the ion exchange column. Vanadium was eluted from the column using 1M hydrochloric acid and injected in the graphite furnace using a mixture of hydrofluoric acid plus magnesium nitrate as chemical modifiers. Calibration was carried out using multiple injection and aqueous standards prepared in the same medium. Detection limits were 0.2 ng g(-1) for infant formulas and 0.02 microg L(-1) for cow milk samples. The reliability of the procedure was checked by comparing the results obtained with those found using a previous mineralization stage and by analyzing five certified reference materials.

  5. Highly efficient single cell arraying by integrating acoustophoretic cell pre-concentration and dielectrophoretic cell trapping.

    PubMed

    Kim, Soo Hyeon; Antfolk, Maria; Kobayashi, Marina; Kaneda, Shohei; Laurell, Thomas; Fujii, Teruo

    2015-11-21

    To array rare cells at the single-cell level, the volumetric throughput may become a bottleneck in the cell trapping and the subsequent single-cell analysis, since the target cells per definition commonly exist in a large sample volume after purification from the original sample. Here, we present a novel approach for high throughput single cell arraying by integrating two original microfluidic devices: an acoustofluidic chip and an electroactive microwell array. The velocity of the cells is geared down in the acoustofluidic chip while maintaining a high volume flow rate at the inlet of the microsystem, and the cells are subsequently trapped one by one into the microwell array using dielectrophoresis. The integrated system exhibited a 10 times improved sample throughput compared to trapping with the electroactive microwell array chip alone, while maintaining a highly efficient cell recovery above 90%. The results indicate that the serial integration of the acoustophoretic pre-concentration with the dielectrophoretic cell trapping drastically improves the performance of the electroactive microwell array for highly efficient single cell analysis. This simple and effective system for high throughput single cell arraying with further possible integration of additional functions, including cell sorting and downstream analysis after cell trapping, has potential for development to a highly integrated and automated platform for single-cell analysis of rare cells.

  6. Preconcentration and Spectrophotometric Determination of a Naphthalene Analog of Medetomidine Using Modified Maghemite Nanoparticles

    NASA Astrophysics Data System (ADS)

    Maddah, B.; Hosseini, F.; Ahmadi, M.; Rajabi, A. Asghar; Beik-Mohammadlood, Z.

    2016-05-01

    A novel and sensitive extraction procedure using sodium dodecyl sulfate (SDS) modified maghemite nanoparticles (MNPs) as an efficient solid phase has been developed for removal, preconcentration, and spectrophotometric determination of trace amounts of a naphthalene analog of dexmedetomidine (4-(1-(na phthalene-1-yl)ethyl)-1Himidazole, NMED). The MNPs were obtained by a coprecipitation method, and their surfaces were furthermore modified by SDS. The size and morphological properties of the synthesized MNPs were determined by X-ray diffraction analysis, FT-IR, vibrating sample magnetometry, and scanning electron microscopy. NMED was adsorbed at pH 3.0. The adsorbed drug was then desorbed and determined by spectrophotometry at 280 nm. The calibration graph was linear in the range 1 × 10-6-1 × 10-4 mol/L of NMED with a correlation coefficient of 0.989. The detection limit of the method for NMED determination was 3.7 × 10-7 mol/L. The method was successfully applied to the determination of NMED in human urine samples.

  7. Online preconcentration of arsenic compounds by dynamic pH junction-capillary electrophoresis.

    PubMed

    Jaafar, Jafariah; Irwan, Zildawarni; Ahamad, Rahmalan; Terabe, Shigeru; Ikegami, Tohru; Tanaka, Nobuo

    2007-02-01

    An online preconcentration technique by dynamic pH junction was studied to improve the detection limit for anionic arsenic compounds by CE. The main target compound is roxarsone, or 3-nitro-4-hydroxyphenylarsonic acid, which is being used as an animal feed additive. The other inorganic and organoarsenic compounds studied are the possible biotransformation products of roxarsone. The arsenic species were separated by a dynamic pH junction in a fused-silica capillary using 15 mM phosphate buffer (pH 10.6) as the BGE and 15 mM acetic acid as the sample matrix. CE with UV detection was monitored at a wavelength of 192 nm. The influence of buffer pH and concentration on dynamic pH junction were investigated. The arsenic species focusing resulted in LOD improvement by a factor of 100-800. The combined use of C18 and anion exchange SPE and dynamic pH junction to CE analysis of chicken litter and soils helps to increase the detection sensitivity. Recoveries of spiked samples ranged between 70 and 72%.

  8. Extraction and preconcentration of hemin from human blood serum and breast cancer supernatant.

    PubMed

    Sedaghat, Somayeh; Shamspur, Tayebeh; Mohamadi, Maryam; Mostafavi, Ali

    2015-12-01

    A green, facile, fast, and sensitive liquid-phase microextraction method is presented for the extraction and preconcentration of hemin in the presence of free iron ions prior to flame atomic absorption spectroscopic determination. In this technique, an anion-functionalized task-specific ionic liquid is used as the extracting solvent. The interface between the extracting solvent and the bulk aqueous phase containing hemin is enormously enlarged by dispersing the ionic liquid to the aqueous phase with the help of ultrasound radiation. Hemin is selectively extracted into the ionic liquid after interaction with the functional group of the ionic liquid. Then, the concentration of the extracted hemin is determined through the absorbance of the iron ions contained in the hemin structure using flame atomic absorption spectroscopy. Different experimental parameters affecting the extraction efficiency have been optimized. Under the optimized conditions, the proposed method has a hemin concentration linear range of 0.020-0.80 mg/L with a detection limit of 0.0080 mg/L. This method has been successfully applied to the extraction and determination of hemin in human serum and supernatant samples. PMID:26496188

  9. An automatic system for on-line flash flood forecasting

    NASA Astrophysics Data System (ADS)

    Makin, I.; Rumyantsev, D.; Shemanayev, K.; Shkarbanov, R.

    2012-04-01

    The research group at Russian State Hydrometeorological University continues developing hydrologic software, called SLS+, which might be useful for background flash flood forecasting in poorly gauged regions. Now the SLS+ software has a user-friendly web interface for on-line background flash flood forecasting in training and operational (real time or near real time) modes, and allows issuing stream flow forecasts based on precipitation and evaporation data obtained either from archives, or from field sensors, respectively. The system currently includes two hydrological models, the Sacramento Soil Moisture Accounting model (USA) and Multi-Layer Conceptual Model (Russia). These models can be calibrated either manually, or automatically based on four calibration algorithms: Shuffled Complex Evolution algorithm (SCE), which is quite useful if (1) a number of calibrated parameters does not exceed 6-7 and boundaries of the parameter space are well defined and (2) the parameter space is not too wide; Basic Stepwise Line Search (SLS) algorithm, which is efficient and computationally "inexpensive", if an initial point for pattern optimization is well defined; SLS-2L algorithm (where 2L is an abbreviation for "two loops" or "two cycles"), which is used in regions with scarce soil data and allows first to predetermine the soil hydraulic parameters, and then use these parameters for the refined model parameterization; SLS-E algorithm (where E stands for "Ensemble generation"), which implies the generation of ensembles of one or several forcing processes (for instance, effective precipitation and evaporation) and model calibration for each of those ensembles. This method is primarily designed for models with undistracted parameters at a relatively low density of ground-based meteorological observation network. Currently the trial version of the system is available for testing upon request.

  10. On-line maintenance methodology development and its applications

    SciTech Connect

    Kim, J.; Jae, M.

    2012-07-01

    With the increasing economic pressures being faced and the potential for shortening outage times under the conditions of deregulated electricity markets in the world, licensees are motivated to get an increasing amount of the on-line maintenance (OLM). The benefits of the OLM includes increased system and plant reliability, reduction of plant equipment and system material condition deficiencies that could adversely impact operations, and reduction of work scope during plant refueling outages. In Korea, allowance guidelines of risk assessment is specified in the safety regulation guidelines 16.7 and 16.8 of the Korea Inst. of Nuclear Safety (KINS), which is 'General guidelines of Risk-informed application for requesting permission of changes' and 'Requesting permission of changes of Risk-informed application for Technical Specification'. We select the emergency diesel generator (EDG) of the Ulchin unit 3 and 4 for risk assessment analysis by applying configuration changes. The EDG which has plant safety level IE belongs to on-site standby power (A, B train EDG) in electric distribution system. The EDG is important component because it should maintain standby status during plant is operating, therefore we select the EDG for target component of risk assessment analysis. The risk assessment is limited to CDF. The risk assessment is performed by using AIMS-PSA Release2. We evaluate CDF by applying the configuration changes with some assumptions. Evaluation of the full power operation and Low power/Shut down operation was performed. This study has been performed for introducing a methodology and performing risk assessment. (authors)

  11. On-line fermentation monitoring by mid-infrared spectroscopy.

    PubMed

    Mazarevica, Gunta; Diewok, Josef; Baena, Josefa R; Rosenberg, Erwin; Lendl, Bernhard

    2004-07-01

    A new method for on-line monitoring of fermentations using mid-infrared (MIR) spectroscopy has been developed. The method has been used to predict the concentrations of glucose and ethanol during a baker's yeast fermentations. A completely automated flow system was employed as an interface between the bioprocess under study and the Fourier transform infrared (FT-IR) spectrometer, which was equipped with a flow cell housing a diamond attenuated total reflection (ATR) element. By using the automated flow system, experimental problems related to adherence of CO(2) bubbles to the ATR surface, as well as formation of biofilms on the ATR surface, could be efficiently eliminated. Gas bubbles were removed during sampling, and by using rinsing steps any biofilm could be removed from the ATR surface. In this way, constant measuring conditions could be guaranteed throughout prolonged fermentation times (approximately 8 h). As a reference method, high-performance liquid chromatography (HPLC) with refractive index detection was used. The recorded data from different fermentations were modeled by partial least-squares (PLS) regression comparing two different strategies for the calibration. On the one hand, calibration sets were constructed from spectra recorded from either synthetic standards or from samples drawn during fermentation. On the other hand, spectra from fermentation samples and synthetic standards were combined to form a calibration set. Differences in the kinetics of the studied fermentation processes used for calibration and prediction, as well as the precision of the HPLC reference method, were identified as the main chemometric sources of error. The optimal PLS regression method was obtained using the mixed calibration set of samples from fermentations and synthetic standards. The root mean square errors of prediction in this case were 0.267 and 0.336 g/L for glucose and ethanol concentration, respectively.

  12. The Eclipsing Binary On-Line Atlas (EBOLA)

    NASA Astrophysics Data System (ADS)

    Bradstreet, D. H.; Steelman, D. P.; Sanders, S. J.; Hargis, J. R.

    2004-05-01

    In conjunction with the upcoming release of \\it Binary Maker 3.0, an extensive on-line database of eclipsing binaries is being made available. The purposes of the atlas are: \\begin {enumerate} Allow quick and easy access to information on published eclipsing binaries. Amass a consistent database of light and radial velocity curve solutions to aid in solving new systems. Provide invaluable querying capabilities on all of the parameters of the systems so that informative research can be quickly accomplished on a multitude of published results. Aid observers in establishing new observing programs based upon stars needing new light and/or radial velocity curves. Encourage workers to submit their published results so that others may have easy access to their work. Provide a vast but easily accessible storehouse of information on eclipsing binaries to accelerate the process of understanding analysis techniques and current work in the field. \\end {enumerate} The database will eventually consist of all published eclipsing binaries with light curve solutions. The following information and data will be supplied whenever available for each binary: original light curves in all bandpasses, original radial velocity observations, light curve parameters, RA and Dec, V-magnitudes, spectral types, color indices, periods, binary type, 3D representation of the system near quadrature, plots of the original light curves and synthetic models, plots of the radial velocity observations with theoretical models, and \\it Binary Maker 3.0 data files (parameter, light curve, radial velocity). The pertinent references for each star are also given with hyperlinks directly to the papers via the NASA Abstract website for downloading, if available. In addition the Atlas has extensive searching options so that workers can specifically search for binaries with specific characteristics. The website has more than 150 systems already uploaded. The URL for the site is http://ebola.eastern.edu/.

  13. Worldwide On-line Distance Learning University Astronomy

    NASA Astrophysics Data System (ADS)

    Eyres, S. P. S.; Hassall, B. J. M.; Butchart, I.; Bromage, G. E.

    2006-08-01

    The University of Central Lancashire operates a suite of distance learning courses in Astronomy, available both on-line and via CD-ROM. The courses are available worldwide, and emphasise flexibility of study. To this end students can study anything from a single module (1/6^th of a full year at degree level) all the way up to an entire degree entirely by distance learning. Study rates vary from one to four modules each year, and students can move on to Level 2 modules (equivalent to second year level in a UK degree) before completing the full set of Level 1 modules. Over 1000 awards have been made to date. The core syllabus is Astronomy and Cosmology at Level 1, alongside skills in literature research, using computers, and basic observing. We also offer a basic history of European astronomy. At Level 2 we look at the astrophysics of the Sun, the stars, and galaxies including the Milky Way. By Level 3 students are expected to engage in a large individual project, and a collaborative investigation with other students, alongside high-level courses in cosmology, relativity, extreme states of matter and the origins of the elements, life and astronomical objects. While many students are retired people looking to exercise their brains, keen amateur amateurs or professionals with disposable incomes, and significant fraction are teachers seeking to improve their subject knowledge or high school students gaining an edge in the UK University entrance competition. Via our involvement with SALT we offer our courses to members of previously disadvantaged communities. This leads to an incredibly diverse and lively student body.

  14. Chitosan modified ordered mesoporous silica as micro-column packing materials for on-line flow injection-inductively coupled plasma optical emission spectrometry determination of trace heavy metals in environmental water samples.

    PubMed

    Chen, Dahui; Hu, Bin; Huang, Chaozhang

    2009-04-30

    A novel adsorbent of chitosan chemically modified ordered mesoporous silica was synthesized and employed as a solid phase extraction (SPE) material for flow injection (FI) micro-column preconcentration on-line coupled with inductively coupled plasma optical emission spectrometry (ICP-OES) determination of trace heavy metals V, Cu, Pb, Cd and Hg in environmental water samples. The factors affecting separation and preconcentration of target heavy metals such as pH, sample flow rate and volume, eluent concentration and volume, interfering ions were investigated. Under the optimized experimental conditions, an enrichment factor of 20 and sampling frequency of 10h(-1) were obtained. The detection limits of the method for V, Cu, Pb, Cd and Hg were 0.33, 0.30, 0.96, 0.05 and 0.93 ng mL(-1), and the relative standard deviations (RSDs) were 2.8%, 6.7%, 1.8%, 4.0% and 5.3% (n=7, C=10 ng mL(-1)), respectively. The adsorption capacities of chitosan modified ordered mesoporous silica for V, Cu, Pb, Cd, and Hg were found to be 16.3, 21.7, 22.9, 12.2 and 13.5 mg g(-1), respectively. In order to validate the developed method, a certified reference material of GSBZ50009-88 environmental water sample was analyzed and the determined values were in good agreement with the certified values. The proposed method has also been applied to the determination of trace heavy metals in natural water samples with satisfactory results.

  15. On-line collection/concentration and determination of transition and rare-earth metals in water samples using Multi-Auto-Pret system coupled with inductively coupled plasma-atomic emission spectrometry.

    PubMed

    Katarina, Rosi Ketrin; Oshima, Mitsuko; Motomizu, Shoji

    2009-05-15

    On-line preconcentration and determination of transition and rare-earth metals in water samples was performed using a Multi-Auto-Pret system coupled with inductively coupled plasma-atomic emission spectrometry (ICP-AES). The Multi-Auto-Pret AES system proposed here consists of three Auto-Pret systems with mini-columns that can be used for the preconcentration of trace metals sequentially or simultaneously, and can reduce analysis time to one-third and running cost of argon gas and labor. A newly synthesized chelating resin, ethylenediamine-N,N,N'-triacetate-type chitosan (EDTriA-type chitosan), was employed in the Multi-Auto-Pret system for the collection of trace metals prior to their measurement by ICP-AES. The proposed resin showed very good adsorption ability for transition and rare-earth metal ions without any interference from alkali and alkaline-earth metal ions in an acidic media. For the best result, pH 5 was adopted for the collection of metal ions. Only 5 mL of samples could be used for the determination of transition metals, while 20 mL of samples was necessary for the determination of rare-earth metals. Metal ions adsorbed on the resin were eluted using 1.5 M nitric acid, and were measured by ICP-AES. The proposed method was evaluated by the analysis of SLRS-4 river water reference materials for trace metals. Good agreement with certified and reference values was obtained for most of the metals examined; it indicates that the proposed method using the newly synthesized resin could be favorably used for the determination of transition and rare-earth metals in water samples by ICP-AES.

  16. On-line preconcentration of niobium(V) and tantalum(V) as 4-(2-pyridylazo) resorcinol-citrate ternary complexes in geological samples by ion interaction high-performance liquid chromatography.

    PubMed

    Vachirapatama, N; Doble, P; Haddad, P R

    2000-07-14

    4-(2-Pyridylazo) resorcinol (PAR) and citrate were used as pre-column complexing agents for the determination of Nb(V) and Ta(V) as ternary complexes in geological samples. Aliquots of 2 ml of the standard and sample solutions containing the Nb(V) and Ta(V) complexes were loaded onto a concentrator column (C18, 0.4 cm x 4.6 mm) with a carrier mobile phase comprising 20% (v/v) methanol and containing 5 mM acetic acid, 5 mM citric acid and 10 mM tetrabutylammonium bromide (TBABr), pH 6.5 at 2 ml/min for 2 min, with the effluent being directed to waste. An automatic switching valve was then switched to flush both complexes from the concentrator column onto a C18 analytical column using a mobile phase comprising 32% (v/v) methanol and containing 5 mM acetic acid, 5 mM citric acid and 3 mM TBABr, pH 6.5 for 2.5 min. The switching valve was then switched back to the original position, and cleaned with methanol for 7 min to eliminate unwanted species still adsorbed to the concentrator column. This procedure prevented later eluting compounds from reaching the analytical column, which reduced the overall run time. The detection limits of Nb(V) and Ta(V) (determined at a signal-to-noise ratio of 3, detection wavelength of 540 nm and a 2-ml sample volume) were 0.012 and 0.039 ppb for Nb(V) and Ta(V), respectively. Recoveries of Nb(V) and Ta(V) were 99.4 and 96.2%, respectively. The HPLC results obtained from the reference granite and basalt samples agreed well with inductively coupled plasma MS and certified values, but the HPLC method yielded slightly low values of the Nb/Ta ratio.

  17. On-line Geoscience Data Resources for Today's Undergraduates

    NASA Astrophysics Data System (ADS)

    Goodwillie, A. M.; Ryan, W.; Carbotte, S.; Melkonian, A.; Coplan, J.; Arko, R.; O'Hara, S.; Ferrini, V.; Leung, A.; Bonckzowski, J.

    2008-12-01

    Broadening the experience of undergraduates can be achieved by enabling free, unrestricted and convenient access to real scientific data. With funding from the U.S. National Science Foundation, the Marine Geoscience Data System (MGDS) (http://www.marine-geo.org/) serves as the integrated data portal for various NSF-funded projects and provides free public access and preservation to a wide variety of marine and terrestrial data including rock, fluid, biology and sediment samples information, underway geophysical data and multibeam bathymetry, water column and multi-channel seismics data. Users can easily view the locations of cruise tracks, sample and station locations against a backdrop of a multi-resolution global digital elevation model. A Search For Data web page rapidly extracts data holdings from the database and can be filtered on data and device type, field program ID, investigator name, geographical and date bounds. The data access experience is boosted by the MGDS use of standardised OGC-compliant Web Services to support uniform programmatic interfaces. GeoMapApp (http://www.geomapapp.org/), a free MGDS data visualization tool, supports map-based dynamic exploration of a broad suite of geosciences data. Built-in land and marine data sets include tectonic plate boundary compilations, DSDP/ODP core logs, earthquake events, seafloor photos, and submersible dive tracks. Seamless links take users to data held by external partner repositories including PetDB, UNAVCO, IRIS and NGDC. Users can generate custom maps and grids and import their own data sets and grids. A set of short, video-style on-line tutorials familiarises users step- by-step with GeoMapApp functionality (http://www.geomapapp.org/tutorials/). Virtual Ocean (http://www.virtualocean.org/) combines the functionality of GeoMapApp with a 3-D earth browser built using the NASA WorldWind API for a powerful new data resource. MGDS education involvement (http://www.marine-geo.org/, go to Education tab

  18. Progressive thermal desorption of vapor mixtures from a preconcentrator with a porous metal foam internal architecture and variable thermal ramp rates.

    PubMed

    Grate, Jay W; Anheier, Norman C; Baldwin, David L

    2005-03-15

    A vapor preconcentrator has been designed with the porous polymer (Tenax) packed into a highly porous metal foam to facilitate thermal conductivity and temperature uniformity throughout the bed of the preconcentrator during heating. Vapors were desorbed using linear temperature programming from room temperature to a maximum temperature of 170 or 200 degrees C; the programmed duration of the thermal ramp was varied from 10 to 180 s. The partial separation of vapor mixtures that are thermally desorbed from the preconcentrator has been examined in terms of a metric for resolution, using methyl ethyl ketone, toluene, and dimethyl methylphosphonate as a test mixture. Vapors desorbed as a sequence of partially separated overlapping peaks, as observed with a polymer-coated flexural plate wave sensor. It was shown that vapor mixture resolution improved as the total time of the thermal ramp was extended from 30 to 120 s. In this way, the preconcentrator serves to act as a preseparator in addition to its usual functions for sampling, signal modulation, and improving sensitivity. Overlapping peaks were modeled, and peak areas were extracted using an exponentially modified Gaussian model. Peak areas were independent of the thermal ramp rate. Uses of such preconcentrators with multivariate detectors, such as sensor arrays, are discussed.

  19. Progressive Thermal Desorption of Vapor Mixtures from a Preconcentrator with a Porous Metal Foam Internal Architecture and Variable Thermal Ramp Rates

    SciTech Connect

    Grate, Jay W.; Anheier, Norman C.; Baldwin, David L.

    2005-03-15

    A vapor preconcentrator has been designed with the porous polymer (Tenax) packed into a highly porous metal foam to facilitate thermal conductivity and temperature uniformity throughout the bed of the preconcentrator during heating. Vapors were desorbed using linear temperature programming from room temperature to a maximum temperature of 170ºC or 200ºC; the programmed duration of the thermal ramp was varied from 10 to 180 seconds. The thermal desorption of vapor mixtures captured on the preconcentrator has been examined in detail, using methyl ethyl ketone, toluene, and dimethyl methylphosphonate as a test mixture. Vapors desorbed as a sequence of partially separated overlapping peaks as observed with a polymer-coated flexural plate wave sensor. It was shown that vapor mixture resolution improved as the total time of the thermal ramp was extended from 30 seconds to 120 seconds. In this way the preconcentrator serves to act as a preseparator in addition to its usual functions for sampling, signal modulation, and improving sensitivity. Overlapping peaks were modeled and peak areas were extracted using an exponentially modified Gaussian model. Peak areas were independent of the thermal ramp rate. Uses of such preconcentrators with multivariate detectors such as sensor arrays are discussed.

  20. Progressive thermal desorption of vapor mixtures from a preconcentrator with a porous metal foam internal architecture and variable thermal ramp rates.

    PubMed

    Grate, Jay W; Anheier, Norman C; Baldwin, David L

    2005-03-15

    A vapor preconcentrator has been designed with the porous polymer (Tenax) packed into a highly porous metal foam to facilitate thermal conductivity and temperature uniformity throughout the bed of the preconcentrator during heating. Vapors were desorbed using linear temperature programming from room temperature to a maximum temperature of 170 or 200 degrees C; the programmed duration of the thermal ramp was varied from 10 to 180 s. The partial separation of vapor mixtures that are thermally desorbed from the preconcentrator has been examined in terms of a metric for resolution, using methyl ethyl ketone, toluene, and dimethyl methylphosphonate as a test mixture. Vapors desorbed as a sequence of partially separated overlapping peaks, as observed with a polymer-coated flexural plate wave sensor. It was shown that vapor mixture resolution improved as the total time of the thermal ramp was extended from 30 to 120 s. In this way, the preconcentrator serves to act as a preseparator in addition to its usual functions for sampling, signal modulation, and improving sensitivity. Overlapping peaks were modeled, and peak areas were extracted using an exponentially modified Gaussian model. Peak areas were independent of the thermal ramp rate. Uses of such preconcentrators with multivariate detectors, such as sensor arrays, are discussed. PMID:15762598

  1. Cetyltrimethylammonium Bromide-coated magnetic nanoparticles for the preconcentration of phenolic compounds from environmental water samples.

    PubMed

    Zhao, Xiaoli; Shi, Yali; Cai, Yaqi; Mou, Shifen

    2008-02-15

    The research presented in this paper investigates the adsorption of cation surfactants--cetyltrimethylammonium bromide (CTAB) and cetylpyridinium chloride (CPC)--onto magnetic nanoparticles and the application of this mixed hemimicelles solid-phase extraction (SPE) method for the preconcentration of several typical phenolic compounds-bisphenol A (BPA), 4-tertoctylphenol (4-OP), and 4-n-nonylphenol (4-NP)--from environmental water samples. In this novel SPE method, the charged surfactants CTAB and CPC form mixed hemimicelles on Fe3O4 nanoparticles (Fe3O4 NPs), which causes retention of analytes by strong hydrophobic and electrostatic interactions. The SPE method combines the advantages of mixed hemimicelles and magnetic nanoparticles. In order to provide guidelines forthe mixed hemimicelles SPE method development, surfactant adsorption isotherms and zeta-potential isotherms were also investigated. The main factors affecting the adsolubilization of analytes, such as the amount of Fe3O4 NPs and surfactants, the type of surfactants, the solution pH,the sample loading volume, and the desorption conditions, were investigated and optimized. A concentration factor of 800 was achieved by the extraction of 800 mL of several environmental water samples using this SPE method. Under the selected conditions, detection limits obtained for BPA, 4-OP, and 4-NP were 12, 29, 34 ng/L, respectively. The accuracy of the method was evaluated by recovery measurements on spiked samples, and good recoveries (68-104%) with low relative standard deviations from 2 to 7% were achieved. The advantages of this new SPE method include high extraction yields, high breakthrough volumes, short analysis times, and easy preparation of sorbents. To the best of our knowledge, this is the first time that a mixed hemimicelles SPE method based on magnetic separation and nanoparticles has been used for the pretreatment of environmental water samples.

  2. Rapid preconcentration for liquid chromatography-mass spectrometry assay of trace level neuropeptides.

    PubMed

    Zhou, Ying; Mabrouk, Omar S; Kennedy, Robert T

    2013-11-01

    Measurement of neuropeptides in the brain through in vivo microdialysis sampling provides direct correlation between neuropeptide concentration and brain function. Capillary liquid chromatography-multistage mass spectrometry (CLC-MS(n)) has proven to be effective at measuring endogenous neuropeptides in microdialysis samples. In the method, microliter samples are concentrated onto nanoliter volume packed beds before ionization and mass spectrometry analysis. The long times required for extensive preconcentration present a barrier to routine use because of the many samples that must be analyzed and instability of neuropeptides. In this study, we evaluated the capacity of 75 μm inner diameter (i.d.) capillary column packed with 10 μm reversed phase particles for increasing the throughput in CLC-MS(n) based neuropeptide measurement. Coupling a high injection flow rate for fast sample loading/desalting with a low elution flow rate to maintain detection sensitivity, this column has reduced analysis time from ∼30 min to 3.8 min for 5 μL sample, with 3 pM limit of detection (LOD) for enkephalins and 10 pM LOD for dynorphin A1-8 in 5 μL sample. The use of isotope-labeled internal standard lowered peptide signal variation to less than 5 %. This method was validated for in vivo detection of Leu and Met enkephalin with microdialysate collected from rat globus pallidus. The improvement in speed and stability makes CLC-MS(n) measurement of neuropeptides in vivo more practical.

  3. Microfabricated passive vapor preconcentrator/injector designed for microscale gas chromatography.

    PubMed

    Seo, Jung Hwan; Kim, Sun Kyu; Zellers, Edward T; Kurabayashi, Katsuo

    2012-02-21

    The design, fabrication, and preliminary testing of a micromachined-Si passive vapor preconcentrator/injector (μPPI) are described. Intended for incorporation in a gas chromatographic microsystem (μGC) for analyzing organic vapor mixtures, the μPPI captures vapors from the air at a known rate by means of passive diffusion (i.e., without pumping) and then desorbs the vapor sample thermally by means of an integrated heater and injects it downstream (with pumping). The μPPI chip comprises a 1.8 μL deep reactive-ion-etched (DRIE) Si cavity with a resistively heated membrane floor and a DRIE-Si cap containing >1500 parallel diffusion channels, each 54 × 54 × 200 μm. The cavity is packed with 750 μg of a commercial graphitized carbon adsorbent. Fluidic and heat-transfer modeling was used to guide the design process to ensure power-efficient sample transfer during thermal desorption. Experiments performed with toluene at concentrations of ~1 ppm gave a constant sampling rate of 9.1 mL min(-1) for up to 30 min, which is within 2% of theoretical predictions and corresponds to a linear dynamic mass uptake range of ~1 μg. The cavity membrane could be heated to 250 °C in 0.23 s with 1 W of applied power and, with 50 mL min(-1) of suction flow provided by a downstream pump, yielded >95% desorption/injection efficiency of toluene samples over an 8-fold range of captured mass.

  4. Determination of bezafibrate, methotrexate, cyclophosphamide, orlistat and enalapril in waste and surface waters using on-line solid-phase extraction liquid chromatography coupled to polarity-switching electrospray tandem mass spectrometry.

    PubMed

    Garcia-Ac, Araceli; Segura, Pedro A; Gagnon, Christian; Sauvé, Sébastien

    2009-04-01

    We developed a rapid method for the monitoring of five selected pharmaceuticals in the influent and effluent of municipal wastewater treatment plants (WWTP) as well as in the effluent-receiving waters. To that end, we optimized and validated an analytical method based on on-line solid-phase extraction (on-line SPE) coupled with reversed-phase liquid chromatography-switching polarity electrospray ionization-tandem mass spectrometry (LC-ESI(+/-)-MS/MS). The target analytes have a variable hydrophobic character and belong to various therapeutic classes including the lipid regulator bezafibrate, the chemotherapy drugs methotrexate and cyclophosphamide, the lipase inhibitor orlistat and the angiotensin converting enzyme (ACE) inhibitor used in the treatment of hypertension, enalapril. The method combines positive and negative voltage switching modes, therefore all analytes can be determined using a single injection and without any reduction in sensitivity. In order to detect traces of these compounds, a preconcentration step before detection is performed by loading 1.00 mL of sample in an on-line SPE cartridge and eluting from the cartridge using a reversed-phase liquid chromatography gradient. Analysis of wastewater and surface water samples was greatly affected by co-eluting matrix compounds, to compensate for matrix effects quantitation was therefore performed using standard additions. Method intra-day precision was less than 6.5% and limits of detection in fortified matrix effluent samples ranged from 9 to 20 ng L(-1). Four of the target pharmaceuticals were detected in the WWTP effluents, enalapril and bezafibrate being the most abundant compounds with concentrations of 35 and 239 ng L(-1), respectively. Concentrations of these same compounds in surface water samples from sites downstream in the St. Lawrence River were 8 and 63 ng L(-1), respectively, which was mainly due to dilution.

  5. Cloud point extraction, preconcentration and spectrophotometric determination of trace amount of manganese(II) in water and food samples.

    PubMed

    Gouda, Ayman A

    2014-10-15

    A new cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to extract manganese(II) from aqueous solution was investigated. The method is based on the complexation reaction of manganese(II) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarin) in the presence of borate buffer at pH 8.5 and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by spectrophotometry at 528nm. The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the analytical characteristics of the method (e.g., limit of detection (LOD), linear range, preconcentration and improvement factors) were obtained. The proposed CPE method showed linear calibration within the range 5.0-200ngmL(-1) of manganese(II) and the limit of detection of the method was 0.8ngmL(-1) with an preconcentration factor of ∼50 when 25mL of sample solution was preconcentrated to 0.5mL. The relative standard deviation (RSD) and relative error were found to be 1.35% and 1.42%, respectively (CMn(II)=150ngmL(-1), n=6) for pure standard solutions. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. The method was applied to the determination of manganese(II) in water and food samples with a recovery for the spiked samples in the range of 95.87-102.5%.

  6. Cloud point extraction, preconcentration and spectrophotometric determination of trace amount of manganese(II) in water and food samples

    NASA Astrophysics Data System (ADS)

    Gouda, Ayman A.

    2014-10-01

    A new cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to extract manganese(II) from aqueous solution was investigated. The method is based on the complexation reaction of manganese(II) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarin) in the presence of borate buffer at pH 8.5 and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by spectrophotometry at 528 nm. The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the analytical characteristics of the method (e.g., limit of detection (LOD), linear range, preconcentration and improvement factors) were obtained. The proposed CPE method showed linear calibration within the range 5.0-200 ng mL-1 of manganese(II) and the limit of detection of the method was 0.8 ng mL-1 with an preconcentration factor of ∼50 when 25 mL of sample solution was preconcentrated to 0.5 mL. The relative standard deviation (RSD) and relative error were found to be 1.35% and 1.42%, respectively (CMn(II) = 150 ng mL-1, n = 6) for pure standard solutions. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. The method was applied to the determination of manganese(II) in water and food samples with a recovery for the spiked samples in the range of 95.87-102.5%.

  7. Determination of trace metal ions by AAS in natural water samples after preconcentration of pyrocatechol violet complexes on an activated carbon column.

    PubMed

    Narin, I; Soylak, M; Elçi, L; Doğan, M

    2000-09-01

    A simple preconcentration method is described for the determination of Cu, Mn, Co, Cd, Pb, Ni and Cr in water samples by flame AAS. Trace metal ions in water were sorbed as pyrocatechol violet complexes on activated carbon column at the pH range of 4-8, then eluted with 1 M HNO(3) in acetone. The effect of major cations and anions of the natural water samples on the sorption of metal ions has been also investigated. The concentration of the metal ions detected after preconcentration was in agreement with the added amount. The present method was found to be applicable to the preconcentration of Cu, Mn, Co, Cd, Pb, Ni and Cr in natural water samples with good results such as R.S.D. from 3 to 8% (N=10) and detection limits under 70 ng l(-1). PMID:18968065

  8. Simple method of determination of copper, mercury and lead in potable water with preliminary pre-concentration by total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Hołyńska, B.; Ostachowicz, B.; Wȩgrzynek, D.

    1996-06-01

    Total reflection X-ray fluorescence spectrometry and chemical pre-concentration procedures have been applied for the analysis of trace concentrations of copper, mercury, and lead in drinking water samples. A simple total reflection module has been used in X-ray measurements. The elements under investigation were pre-concentrated by complexation using a mixture of carbamates followed by solvent extraction with methyl isobutyl ketone. The preconcentration procedure was tested with the use of twice-distilled water samples and samples of mineral and tap water spiked with known additions of copper, mercury, and lead. The obtained recovery and precision values are presented. The minimum detection limits for the determination of these elements in mineral and tap water samples were found to be 40 ng l -1, 60 ng l -1, and 60 ng l -1, respectively.

  9. Performance of the goulden large-sample extractor in multiclass pesticide isolation and preconcentration from stream water

    USGS Publications Warehouse

    Foster, G.D.; Foreman, W.T.; Gates, Paul M.

    1991-01-01

    The reliability of the Goulden large-sample extractor in preconcentrating pesticides from water was evaluated from the recoveries of 35 pesticides amended to filtered stream waters. Recoveries greater than 90% were observed for many of the pesticides in each major chemical class, but recoveries for some of the individual pesticides varied in seemingly unpredictable ways. Corrections cannot yet be factored into liquid-liquid extraction theory to account for matrix effects, which were apparent between the two stream waters tested. The Goulden large-sample extractor appears to be well suited for rapid chemical screening applications, with quantitative analysis requiring special quality control considerations. ?? 1991 American Chemical Society.

  10. On-line coupling of Micro-Extraction by Packed Sorbent with Sequential Injection Chromatography system for direct extraction and determination of betaxolol in human urine.

    PubMed

    Šrámková, Ivana; Chocholouš, Petr; Sklenářová, Hana; Šatínský, Dalibor

    2015-10-01

    A novel approach for automation of Micro-Extraction by Packed Sorbent (MEPS), a solid phase extraction technique, is presented, enabling precise and repeatable liquid handling due to the employment of sequential injection technique. The developed system was used for human urine sample clean-up and pre-concentration of betaxolol before its separation and determination. A commercial MEPS C-18 cartridge was integrated into an SIChrom™ system. The chromatographic separation was performed on a monolithic High Resolution C18 (50×4.6 mm) column which was coupled on-line in the system with Micro-Extraction using an additional selection valve. A mixture of acetonitrile and aqueous solution of 0.5% triethylamine with acetic acid, pH adjusted to 4.5 in ratio 30:70 was used as a mobile phase for elution of betaxolol from MEPS directly onto the monolithic column where the separation took place. Betaxolol was quantified by a fluorescence detector at wavelengths λ(ex)=220 nm and λ(em)=305 nm. The linear calibration range of 5-400 ng mL(-1), with limit of detection 1.5 ng mL(-1) and limit of quantification 5 ng mL(-1) and correlation r=0.9998 for both the standard and urine matrix calibration were achieved. The system recovery was 105±5%; 100±4%; 108±1% for three concentration levels of betaxolol in 10 times diluted urine - 5, 20 and 200 ng mL(-1), respectively.

  11. On-line coupling of dynamic microwave-assisted extraction to solid-phase extraction for the determination of sulfonamide antibiotics in soil.

    PubMed

    Chen, Ligang; Zeng, Qinglei; Wang, Hui; Su, Rui; Xu, Yang; Zhang, Xiaopan; Yu, Aimin; Zhang, Hanqi; Ding, Lan

    2009-08-26

    A rapid technique based on dynamic microwave-assisted extraction (DMAE) coupled on-line with solid-phase extraction (SPE) was developed for the determination of sulfonamides (SAs) including sulfadiazine, sulfameter, sulfamonomethoxine and sulfaquinoxaline in soil. The SAs were first extracted with acetonitrile under the action of microwave energy, and then directly introduced into the SPE column which was packed with neutral alumina for preconcentration of analytes and clean-up of sample matrix. Subsequently, the SAs trapped on the alumina were eluted with 0.3% acetic acid aqueous solution and determined by liquid chromatography-tandem mass spectrometry. The DMAE parameters were optimized by the Box-Behnken design. Maximum extraction efficiency was achieved using 320 W of microwave power; 12 mL of extraction solvent and 0.8 mL min(-1) of extraction solvent flow rate. The limits of detection and quantification obtained are in the range of 1.4-4.8 ng g(-1) and 4.6-16.0 ng g(-1) for the SAs, respectively. The mean values of relative standard deviation of intra- and inter-day ranging from 2.7% to 5.3% and from 5.6% to 6.7% are obtained, respectively. The recoveries of SAs obtained by analyzing four spiked soil samples at three fortified levels (20 ng g(-1), 100ngg(-1) and 500 ng g(-1)) were from 82.6+/-6.0% to 93.7+/-5.5%. The effect of standing time of spiked soil sample on the SAs recoveries was examined. The recoveries of SAs decreased from (86.3-101.9)% to (37.6-47.5)% when the standing time changed from one day to four weeks. PMID:19646585

  12. Study of immobilized metal affinity chromatography sorbents for the analysis of peptides by on-line solid-phase extraction capillary electrophoresis-mass spectrometry.

    PubMed

    Ortiz-Martin, Lorena; Benavente, Fernando; Medina-Casanellas, Silvia; Giménez, Estela; Sanz-Nebot, Victoria

    2015-03-01

    Several commercial immobilized metal affinity chromatography sorbents were evaluated in this study for the analysis of two small peptide fragments of the amyloid β-protein (Aβ) (Aβ(1-15) and Aβ(10-20) peptides) by on-line immobilized metal affinity SPE-CE (IMA-SPE-CE). The performance of a nickel metal ion (Ni(II)) sorbent based on nitrilotriacetic acid as a chelating agent was significantly better than two copper metal ion (Cu(II)) sorbents based on iminodiacetic acid. A BGE of 25 mM phosphate (pH 7.4) and an eluent of 50 mM imidazole (in BGE) yielded a 25-fold and 5-fold decrease in the LODs by IMA-SPE-CE-UV for Aβ(1-15) and Aβ(10-20) peptides (0.1 and 0.5 μg/mL, respectively) with regard to CE-UV (2.5 μg/mL for both peptides). The phosphate BGE was also used in IMA-SPE-CE-MS, but the eluent needed to be substituted by a 0.5% HAc v/v solution. Under optimum preconcentration and detection conditions, reproducibility of peak areas and migration times was acceptable (23.2 and 12.0%RSD, respectively). The method was more sensitive for Aβ(10-20) peptide, which could be detected until 0.25 μg/mL. Linearity for Aβ(10-20) peptide was good in a narrow concentration range (0.25-2.5 μg/mL, R(2) = 0.93). Lastly, the potential of the optimized Ni(II)-IMA-SPE-CE-MS method for the analysis of amyloid peptides in biological fluids was evaluated by analyzing spiked plasma and serum samples. PMID:25640944

  13. Separation and Preconcentration of Sudan Blue II Using Membrane Filtration and UV-Visible Spectrophotometric Determination in River Water and Industrial Wastewater Samples.

    PubMed

    Unsal, Yunus Emre; Tuzen, Mustafa; Soylak, Mustafa

    2015-01-01

    A new separation and preconcentration method based on adsorption on a cellulose acetate membrane filter and elution with ethanol was established for the UV-Vis spectrophotometric determination of Sudan blue II. Various analytical parameters such as pH of working media, flow rates of solutions, and sample volumes were optimized. Matrix effects of concomitants were investigated for the quantitative recovery values of Sudan blue II. The preconcentration factor was 200. LOD was calculated as 0.96 μg/L. RSD was 5.1%. The optimized procedure was applied to the spectrophotometric determination of Sudan blue II in river and industrial wastewater samples from oil and dye products.

  14. Mesoporous Silica Nanoparticles as an Adsorbent for Preconcentration and Determination of Trace Amount of Nickel in Environmental Samples by Atom Trap Flame Atomic Absorption Spectrometry

    NASA Astrophysics Data System (ADS)

    Shirkhanloo, H.; Falahnejad, M.; Zavvar Mousavi, H.

    2016-01-01

    A rapid enrichment method based on solid-phase extraction (SPE) has been established for preconcentration and separation of trace Ni(II) ions in water samples prior to their determination by atom trap flame atomic absorption spectrometry. A column filled with bulky NH2-UVM7 was used as the novel adsorbent. Under optimal conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were 3-92 μg/L, 0.8 μg/L, and 100, respectively. The validity of the method was checked by the standard reference material.

  15. A Survey of Five On-line Retrieval Systems. Final Report.

    ERIC Educational Resources Information Center

    Welch, Noreen O.

    This report is a survey of five on-line retrieval systems that, with one exception, have been used to demonstrate on-line access to the recently developed Committee on Scientific and Technical Information (COSATI) inventory of government sponsored work now in progress in the area of information sciences and technology. The report was prepared to…

  16. Students Reflecting on Test Performance and Feedback: An On-Line Approach

    ERIC Educational Resources Information Center

    Fyfe, Georgina; Fyfe, Sue; Meyer, Jan; Ziman, Mel; Sanders, Kathy; Hill, Julie

    2014-01-01

    Undergraduate students accessing on-line tests in Human Biology in three Western Australian universities were asked to complete an on-line post-test reflective survey about their perceptions of their test performance in light of automated feedback. The survey allowed pre-determined choices and comment text boxes relating to students'…

  17. On-Line Literature: The Challenge of Integrating Web-Based Materials

    ERIC Educational Resources Information Center

    Ruzich, Constance M.

    2012-01-01

    This classroom research discusses the challenges of integrating face-to-face interactions with the use of on-line resources in secondary English classrooms. Examining the lesson plans of pre-service and early career teachers in the US, I found that the uses of on-line resources were frequently neither coherent nor consistent with the goals and…

  18. The Impact of Cognitive Style on Social Networks in On-Line Discussions

    ERIC Educational Resources Information Center

    Jablokow, Kathryn; Vercellone-Smith, Pamela

    2011-01-01

    With the rise of e-Learning in engineering education, understanding the impact of individual differences on the ways students communicate and collaborate on-line has become increasingly important. The research described here investigates the influence of cognitive style on the interactions within student social networks in an on-line learning…

  19. On-Line IDCMS Delivery of Different Types of Stimulus Sequences.

    ERIC Educational Resources Information Center

    Follettie, Joseph F.

    On line presentation of the items of a given stimulus sequence may or may not require on line retrieval of items and composition of the sequence. This paper sketches a preliminary taxonomy for auditory, visual, and mixed auditory stimulus sequences. It preliminarily assesses the capability of the Southwest Regional Laboratory Instructional…

  20. An On-Line Electronics Graphics Symbol Set for the PLATO IV System.

    ERIC Educational Resources Information Center

    McClintock, Peggy A.; Kimberlin, Donald A.

    An electronics graphic symbol set for on-line construction of electrical and electronics schematic diagrams is described. Specific procedures involving off-line and on-line activities are presented for the development and entry of schematic diagrams utilizing a stored set of symbols. An example of the commands and coding required for the…

  1. High School Open On-Line Courses (HOOC): A Case Study from Italy

    ERIC Educational Resources Information Center

    Canessa, Enrique; Pisani, Armando

    2013-01-01

    The first implementation of complete high school, open on-line courses (HOOC) aiming to support the training and basic scientific knowledge of young students from the Liceo Ginnasio Dante Alighieri in Gorizia, Italy, is discussed. Using the open source and automated recording system openEyA, HOOC give a student the opportunity to watch on-line, at…

  2. College Students' Choice Modeling of Taking On-Line International Business Courses

    ERIC Educational Resources Information Center

    Yeh, Robert S.

    2006-01-01

    To understand students' choice behavior of taking on-line international business courses, a survey study is conducted to collect information regarding students' actual choices of taking on-line courses and potential factors that may have impacts on students' choices of online learning. Potential factors such as enrollment status, demographic…

  3. The Anatomy of Program Design for an On-Line Business Management Course

    ERIC Educational Resources Information Center

    Barger, Bonita

    2008-01-01

    How does one design an on-line course to bridge theory and practice? How can the feedback of on-going stakeholder (student and administration) be incorporated into the design process to enhance quality? This paper presents the theoretical underpinning of designing an on-line management course recognized as best practice for a "well organized…

  4. On-Line Literature Search and Full Articles in the NASA ADS

    NASA Technical Reports Server (NTRS)

    Eichhorn, G.; Accomazzi, A.; Grant, C. S.; Kurtz, M. J.; Murray, S. S.

    2001-01-01

    The ADS provides free world-wide on-line access to over 2.2 million abstracts and over 1 million scanned pages of the astronomical and planetary literature plus over 4 million links to other relevant on-line information at http://ads.harvard.edu. Additional information is contained in the original extended abstract.

  5. Case Study: Collaborative Creation of an On-Line Degree Program

    ERIC Educational Resources Information Center

    Stewart, Barbara L.; Norwood, Marcella; Ezell, Shirley; Waight, Consuelo

    2006-01-01

    Faculty collaboratively developed an on-line Bachelor of Science degree in Consumer Science and Merchandising (CSM). Part-time faculty and technical support services supported the four-member team. Small grants assisted in the creation and redesign of all CSM major courses for on-line delivery. Issues of appropriate learning strategies, student…

  6. BROWSER: An Automatic Indexing On-Line Text Retrieval System. Annual Progress Report.

    ERIC Educational Resources Information Center

    Williams, J. H., Jr.

    The development and testing of the Browsing On-line With Selective Retrieval (BROWSER) text retrieval system allowing a natural language query statement and providing on-line browsing capabilities through an IBM 2260 display terminal is described. The prototype system contains data bases of 25,000 German language patent abstracts, 9,000 English…

  7. Interactive On-Line Continuing Medical Education: Physicians' Perceptions and Experiences

    ERIC Educational Resources Information Center

    Sargeant, Joan; Curran, Vernon; Jarvis-Selinger, Sandra; Ferrier, Suzanne; Allen, Michael; Kirby, Frances; Ho, Kendall

    2004-01-01

    Introduction: Although research in continuing medical education (CME) demonstrates positive outcomes of on-line CME programs, the effectiveness of and learners' satisfaction with interpersonal interaction in on-line CME are lower. Defined as faculty-learner or learner-learner interpersonal interaction, this study explores physicians' perceptions…

  8. Enhancing On-Line Teaching with Verbal Immediacy through Self-Determination Theory

    ERIC Educational Resources Information Center

    Furlich, Stephen A.

    2013-01-01

    This paper explores the use of instructor verbal immediacy behaviors for on-line classes. Specifically, it demonstrates how instructor verbal immediacy behaviors found in face-to-face classes can also be displayed for on-line classes. It is argued that self-determination theory describes identification of the student as an important role in the…

  9. Improvement plans for the RHIC/AGS on-line model environments

    SciTech Connect

    Brown,K.A.; Ahrens, L.; Beebe-Wang, J.; Morris, J.; Nemesure, S.; Robert-Demolaize, G.; Satogata, T.; Schoefer, V.; Tepikian, S.

    2009-08-31

    The on-line models for Relativistic Ion Collider (RHIC) and the RHIC pre-injectors (the AGS and the AGS Booster) can be thought of as containing our best collective knowledge of these accelerators. As we improve these on-line models we are building the framework to have a sophisticated model-based controls system. Currently the RHIC on-line model is an integral part of the controls system, providing the interface for tune control, chromaticity control, and non-linear chromaticity control. What we discuss in this paper is our vision of the future of the on-line model environment for RHIC and the RHIC preinjectors. Although these on-line models are primarily used as Courant-Snyder parameter calculators using live machine settings, we envision expanding these environments to encompass many other problem domains.

  10. A new spectrophotometric method for determination of selenium in cosmetic and pharmaceutical preparations after preconcentration with cloud point extraction.

    PubMed

    Soruraddin, Mohammad Hosein; Heydari, Rouhollah; Puladvand, Morteza; Zahedi, Mir Mehdi

    2011-01-01

    A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV) was described. In this method, all selenium spices reduced to selenium (IV) using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV) in aqueous solution. The proposed method is based on the complexation of Selenium (IV) with dithizone at pH < 1 in micellar medium (Triton X-100). After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm) and dithizone (434 nm) overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL(-1); the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL(-1) of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples. PMID:21647287

  11. Preconcentration of trace uranium from seawater with solid phase extraction followed by differential pulse polarographic determination in chloroform eluate.

    PubMed

    Dojozan, D; Pournaghi-Azar, M H; Toutounchi-Asr, J

    1998-05-01

    In the present study, an effective method is presented for the separation and preconcentration of uranium (VI) by solid phase extraction (SPE). For this purpose, U(VI) oxinate is formed by the reaction of U(VI) with 8-hydroxyquinoline and adsorbed onto the octylsilane (C-8) SPE cartridge. The analyte is completely eluted with chloroform and determined by differential pulse polarography. The SPE conditions were optimized by evaluating the effective factors such as pH, oxine concentration, type and concentration of buffer and masking agent. By the proposed method a preconcentration factor more than 100 was achieved. The average recovery of uranium (VI) oxinate (0.1 mg l(-1)) was 99.8%. The relative standard deviation was 1.6% for seven replicate determinations of uranyl ion in the solution with a concentration 20 mug l(-1). Some concomitant ions such as Ca(+2), Mg(+2) and Fe(+3) which interfere in extraction or determination process of uranium were masked with EDTA in aqueous phase during the extraction process. The proposed method was successfully used for the determination of uranium in Caspian Sea and Persian Gulf water samples. PMID:18967134

  12. Selective preconcentration of uranyl ion by silica gel phases modified with chelating compounds as inorganic polymeric ion exchangers.

    PubMed

    Mahmoud, Mohamed E; Kenawy, Ibrahim M M; Soliman, Ezzat M; Hafez, Medhat A; Akl, Magda A A; Lashein, Rabab R A

    2008-03-01

    Four chemically modified chelating silica gel phases (I - IV) with ion exchange groups were tested for their potential capability to selectively bind, extract and preconcentrate uranyl ions (UO(2)(2+)) from different aqueous solutions as well as ore samples. Factors affecting such determination processes were studied and optimized. These included the pH of the contact solution, the mass of the silica gel phase extractant, the stirring time during the application of a static technique and the eluent concentration for desorption of the surface-bound uranyl ion and interfering anions and cations. All these factors were evaluated on the basis of determinations of the distribution coefficient value (K(d)) and the percent recovery (R%). Percent recovery values of 91% for silica phase (II) and 93% for silica phase (IV) were identified in the optimum conditions. The proposed preconcentration method was further applied to uranium ore samples as well as granite samples. The determined percentage and ppm values are in good agreement with the standard assigned ones. The structure of the synthesized silica gel phases (I - IV) and their uranyl bound complexes were identified and characterized by means of infrared analysis, thermal analysis (TGA) and potentiometric titration.

  13. Preconcentration and Speciation of Trace Elements and Trace-Element Analogues of Radionuclides by Neutron Activation Analysis

    SciTech Connect

    Chatt, A.

    1999-11-14

    We have developed a number of preconcentration neutron activation analysis (PNAA) methods in our laboratory for the determination of trace elements in a variety of complex sample matrices. We developed a number of cocrystallization and coprecipitation methods for the determination of trace elements in water samples. We developed several methods for the determination of I in foods and diets. We have developed a number of PNAA methods in our laboratory We determined As and Sb in geological materials and natural waters by coprecipitation with Se and Au in silicate rocks and ores by coprecipitation with Te followed by NAA. We developed an indirect NAA method for the determination of B in leachates of borosilicate glass. We have been interested in studying the speciation of Am, Tc, and Np in simulated vitrified groundwater leachates of high-level wastes under oxid and anoxic conditions using a number of techniques. We then used PNAA methods to study speciation of trace-element analogues of radionuclides. We have been able to apply biochemical techniques and NAA for the separation, preconcentration, and characterization of metalloprotein and protein-bound trace-element species in subcellular fractions of bovine kidneys. Lately, we have concentrated our efforts to develop chemical and biochemical methods in conjunction with NAA, NMR, and MS for the separation and identification of extractable organohalogens (EOX) in tissues of beluga whales, cod, and northern pink shrimp

  14. A New Spectrophotometric Method for Determination of Selenium in Cosmetic and Pharmaceutical Preparations after Preconcentration with Cloud Point Extraction

    PubMed Central

    Soruraddin, Mohammad Hosein; Heydari, Rouhollah; Puladvand, Morteza; Zahedi, Mir Mehdi

    2011-01-01

    A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV) was described. In this method, all selenium spices reduced to selenium (IV) using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV) in aqueous solution. The proposed method is based on the complexation of Selenium (IV) with dithizone at pH < 1 in micellar medium (Triton X-100). After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm) and dithizone (434 nm) overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL−1; the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL−1 of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples. PMID:21647287

  15. Combined pre-concentration and real-time in-situ chemical detection of explosives in the marine environment

    NASA Astrophysics Data System (ADS)

    Dock, Matthew L.; Harper, Ross J.; Knobbe, Ed

    2010-04-01

    ICx Nomadics has developed the first known real-time sensor system that is capable of detecting chemical signatures emanating from underwater explosives, based upon the same amplifying fluorescent polymer (AFP) fluorescence-quenching transduction mechanism that the Fido® family of explosives detectors utilizes. The SeaPup is capable of real-time detection of the trace chemical signatures emanating from submerged explosive compounds and has been successfully tested on various marine platforms, including a crawler robot, an autonomous underwater vehicle (AUV), and a remotely operated underwater vehicle (ROV). The present work is focused on advances in underwater in-situ chemical sensing; wherein trace amounts of dissolved explosive compounds may be detected and discriminated from other chemical species found in the marine environment. Recent progress with the SeaPup platform have focused on increasing the sensitivity of the AFP matrix through the development of a preconcentration system designed to harvest explosive analytes from a larger sample volume over a predetermined period of time. This permits real time monitoring of chemical plumes during the approach to a potential source, combined with the lowered limit of detection from extended sampling of targeted items. SeaPup has been shown to effectively map "explosive scent plumes" emanating from an underwater source of TNT, and the preconcentration system has previously been demonstrated to enhance sensitivity be over 2 orders of magnitude in a time window of minutes.

  16. Trace level determination of beryllium in natural and flavored mineral waters after pre-concentration using activated carbon.

    PubMed

    Kılınç, Ersin; Bakırdere, Sezgin; Yaman, Mehmet

    2011-04-01

    The concentrations of beryllium (Be) in natural and flavored mineral water samples were determined by flame atomic absorption spectrophotometer (FAAS) after pre-concentration based on the complexation of Be(+2) with a mixture of acetylacetone (pentane-2,4-dione) plus morin (3,5,7,2',4'-pentaoxyflavone) and adsorption on activated carbon. The adsorbed complex was eluted with 1.5 ml of 2.0 M HNO(3) and evaporated to dryness. After adding 1.5 ml of 2 M HNO(3) and centrifuging, Be in acid solution was determined by FAAS. To remove a number of metals present in water, EDTA was used as a chelating agent. Beryllium in mineral water samples was pre-concentrated by 500-fold, taking 750 ml as initial sample and 1.5 ml as the final volume. The relative standard deviations were sufficiently low for practical purposes and recoveries were up to 85%. Spiking experiments were performed in real samples to establish accuracy and recoveries. The limits of detection and quantification were 0.01 and 0.03 ng ml(-1), respectively. Twenty samples were analyzed for their beryllium content using optimum parameters. The highest concentration of beryllium was found to be 0.94 ± 0.15 ng ml(-1) in a natural mineral water, while beryllium was not detected in five samples.

  17. Selective preconcentration of uranyl ion by silica gel phases modified with chelating compounds as inorganic polymeric ion exchangers.

    PubMed

    Mahmoud, Mohamed E; Kenawy, Ibrahim M M; Soliman, Ezzat M; Hafez, Medhat A; Akl, Magda A A; Lashein, Rabab R A

    2008-03-01

    Four chemically modified chelating silica gel phases (I - IV) with ion exchange groups were tested for their potential capability to selectively bind, extract and preconcentrate uranyl ions (UO(2)(2+)) from different aqueous solutions as well as ore samples. Factors affecting such determination processes were studied and optimized. These included the pH of the contact solution, the mass of the silica gel phase extractant, the stirring time during the application of a static technique and the eluent concentration for desorption of the surface-bound uranyl ion and interfering anions and cations. All these factors were evaluated on the basis of determinations of the distribution coefficient value (K(d)) and the percent recovery (R%). Percent recovery values of 91% for silica phase (II) and 93% for silica phase (IV) were identified in the optimum conditions. The proposed preconcentration method was further applied to uranium ore samples as well as granite samples. The determined percentage and ppm values are in good agreement with the standard assigned ones. The structure of the synthesized silica gel phases (I - IV) and their uranyl bound complexes were identified and characterized by means of infrared analysis, thermal analysis (TGA) and potentiometric titration. PMID:18332547

  18. Determination of rare earth elements in natural water samples - A review of sample separation, preconcentration and direct methodologies.

    PubMed

    Fisher, Andrew; Kara, Derya

    2016-09-01

    This review discusses and compares the methods given for the determination of rare earth elements (REE) in natural water samples, including sea, river, lake, tap, ground and waste waters as well as Antarctic ice. Since REE are at very low concentrations in natural waters, numerous different preconcentration methods have been proposed to enable their measurement. These include liquid liquid extraction, dispersive liquid-liquid micro-extraction and solidified floating drop micro-extraction. In addition to liquid-liquid extraction methods, solid phase extraction using commercial resins, resins made in-house, silica-based exchange materials and other solid media is also discussed. These and other techniques such as precipitation/co-precipitation and flotation are compared in terms of speed, preconcentration factors achieved, precision, accuracy and limits of detection (LOD). Some papers have discussed the direct determination of REE in these sample types. Some have used specialised sample introduction systems such as ultrasonic nebulization whereas others have used a standard sample introduction system coupled with inductively coupled plasma mass spectrometry (ICP-MS) detection. These direct methods have also been discussed and compared. PMID:27543012

  19. Determination of toxic heavy metals in sea water by FAAS after preconcentration with a novel chelating resin.

    PubMed

    Manivannan, D; Biju, V M

    2011-01-01

    A solid phase extraction procedure was developed for preconcentration of toxic heavy metals such as cadmium, cobalt, copper, manganese, lead and zinc in sea water samples. A microcolumn packed with 6-[(4-hydroxyphenyl)diazenyl]naphthalene-2,3-diol-formaldehyde (HPDN-F) resin acts as a sorbent to retain the analyte ions by forming metal chelates. The retained trace level metal was subsequently eluted with 1 mol/L HCl and the acid eluent was analysed by Flame Atomic Absorption Spectrophotometer (FAAS). The HPDN-F chelating resin and its metal chelates were characterized by spectral and thermal analysis. The chelating property of the HPDN-F resin towards divalent metal ions was studied as a function of pH and preconcentration flow rate. The recoveries of cadmium, cobalt, copper, manganese, lead and zinc under the optimum working conditions were above 95%. The relative standard deviations were < 2%. The limits of detection were < 0.1 microg/L. The method presented was applied for the determination of cadmium, cobalt, copper, manganese, lead and zinc in sea water samples.

  20. Determination of trace amounts of zinc by flame atomic absorption spectrometry after preconcentration with modified clinoptilolite zeolite.

    PubMed

    Hajialigol, Saeed; Taher, Mohammad Ali; Malekpour, Akbar

    2008-01-01

    Natural clinoptilolite was used as a sorbent material for solid-phase extraction and preconcentration of zinc. Clinoptilolite was first saturated with cadmium (II) and then modified with benzyldimethyltetradecylammonium chloride for increasing adsorption of 3-(2-arsenophenylazo)-4,5-dihydroxy-2,7-naphthalene disulfonic acid (neothorin). Zinc was quantitatively retained on the adsorbent by the column method in the pH range of 3.8-4.2 at a flow rate of 1 mL/min. It was eluted from the column with 5.0 mL 2 M nitric acid solution at a flow rate of 1 mL/min and determined by flame atomic absorption spectrometry at 213.9 nm. Zinc could be concentrated from a 0.03 microg/L solution with a preconcentration factor of 170. Relative standard deviation for 8 replicate determinations of 2.5 microg zinc in the final solution was 0.92%. The interference of a large number of anions and cations was studied in detail to optimize the conditions, and the method was successfully applied for determination of zinc in standard and real water samples. PMID:19202807

  1. Separation and preconcentration of trace manganese from various samples with Amberlyst 36 column and determination by flame atomic absorption spectrometry.

    PubMed

    Kendüzler, Erdal; Türker, A Rehber; Yalçınkaya, Ozcan

    2006-06-15

    This work assesses the potential of a new adsorptive material, Amberlyst 36, for the separation and preconcentration of trace manganese(II) from various media. It is based on the sorption of manganese(II) ions onto a column filled with Amberlyst 36 cation exchange resin, followed by the elution with 5mL of 3mol/L nitric acid and determination by flame atomic absorption spectrometry (FAAS) without interference of the matrix. Different factors including pH of sample solution, sample volume, amount of resin, flow rate of sample solution, volume and concentration of eluent, and matrix effects for preconcentration were investigated. Good relative standard deviation (3%) and high recovery (>95%) at 100mug/L and high enrichment factor (200) and low analytical detection limit (0.245mug/L) were obtained. The adsorption equilibrium was described well by the Langmuir isotherm model with maximum adsorption capacity of 88mg/g of manganese on the resin. The method was applied for the manganese determination by FAAS in tap water, commercial natural drinking water, commercial treated drinking water and commercial tea bag sample. The accuracy of the method is confirmed by analyzing the certified reference material (tea leaves GBW 07605). The results demonstrated good agreement with the certified values. PMID:18970645

  2. Application of factorial design in optimization of preconcentration procedure for copper determination in soft drink by flame atomic absorption spectrometry.

    PubMed

    Castro, Martha T P O; Baccan, Nivaldo

    2005-03-15

    In the present paper, a procedure for preconcentration and determination of copper in soft drink using flame atomic absorption spectrometry (FAAS) is proposed, which is based on solid-phase extraction of copper(II) ions as its ion pair of 1,10-phenanthroline complexes with the anionic surfactant sodium dodecil sulphate (SDS), by Amberlite XAD-2 resin. The optimization process was carried out using 2(4-1) factorial and 2(2) factorial with a center point designs. Four variables (XAD-2 mass, copper mass, sample flow rate and elution flow rate) were regarded as factors in the optimization. Student's t-test on the results of the 2(4-1) factorial design with eight runs for copper extraction, demonstrated that the factors XAD-2 mass and sample flow rate in the levels studied are statistically significant. The 2(2) factorial with a center point design was applied in order to determine the optimum conditions for extraction. The procedure proposed allowed the determination of copper with detection limits (3alpha/S) of 3.9mugl(-1). The precision, calculated as relative standard deviation (R.S.D.) was 1.8% for 20.0mugl(-1) of copper. The preconcentration factor was 100. The robustness of this procedure is demonstrated by the recovery achieved for determination of copper in the presence of several cations. This procedure was applied to the determination of copper in soft drink samples collected in Campinas, SP, Brazil. PMID:18969940

  3. CZE separation of amitrol and triazine herbicides in environmental water samples with acid-assisted on-column preconcentration.

    PubMed

    Arribas, Alberto Sánchez; Moreno, Mónica; Bermejo, Esperanza; Zapardiel, Antonio; Chicharro, Manuel

    2011-01-01

    A simple analytical scheme for the detection and quantification of amitrol and triazine herbicides (atrazine, ametryn and atraton) and degradation product (2-hydroxyatrazine) in environmental water samples by CZE is reported. On-column preconcentration of analytes from untreated water samples (mineral, spring, tap and river water) is accomplished by introducing an acid plug (200 mM citrate of pH 2.0) after the sample and then proceeding with the CZE separation, using 100 mM formiate buffer of pH 3.5 as running buffer and 25.0 KV as separation voltage. UV detection at 200 nm provides LODs from 50 to 300 nM in untreated samples and they were lowered tenfold by sample preconcentration by evaporation. Calculated recoveries were typically higher than 90%. Minimal detectable concentration of the electroactive amitrol could be decreased about 20-fold when electrochemical detection was employed by monitoring the amperometric signal at +800 mV using a carbon paste electrode (LOD of 9.6 nM, 0.81 μg/L, versus 170 nM, 14.3 μg/L, using amperometric and UV detection, respectively) in untreated water samples.

  4. Separation/preconcentration and determination of cadmium ions by solidification of floating organic drop microextraction and FI-AAS.

    PubMed

    Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Kamranzadeh, Elahe

    2009-09-15

    A simple and selective method for the separation and preconcentration of cadmium in water samples based on solidified floating organic drop microextraction (SFODME) was developed. The cadmium ion in aqueous solution was converted to CdI(4)(2-) and was then extracted with 160 microL of 1-undecanol containing cationic surfactant of methyltrioctylammonium chloride (0.2 mol/L). When the extraction was completed, the sample vial was cooled in an ice bath for 5 min. The solidified extract was transferred into a conical vial where it melted immediately. It was then diluted to 250 microL upon addition of ethanol, and 100 microL of it was analyzed by flow injection flame atomic absorption spectrometry (FI-FAAS). Factors that influence the extraction and ion pair formation, such as pH, concentration of iodide and methyltrioctylammonium chloride, extraction time, sample volume, and ionic strength were optimized. Under the optimized conditions, a preconcentration factor of 640, detection limit of 0.0079 microg/L and good relative standard deviation of +/-5.4% at 5 microg/L were obtained. The procedure was applied to tap water, well water, and sea water; and accuracy was assessed through recovery experiment and independent analysis by graphite atomic absorption spectrometry. The accuracy was also evaluated through analyses of certified reference ore. PMID:19615509

  5. Extraction and preconcentration of trace amounts of diazinon and fenitrothion from environmental water by magnetite octadecylsilane nanoparticles.

    PubMed

    Maddah, Bozorgmehr; Shamsi, Javad

    2012-09-21

    In this study, a method for extraction and preconcentration trace amounts of organophosphorus pesticides (OPPs) in environmental water was developed using magnetic solid phase extraction (magnetic-SPE) followed by high performance liquid chromatography (HPLC) with UV detection. Magnetite octadecylsilane nanoparticles were synthesized and characterized by X-ray diffraction, FTIR spectroscopy, vibrating sample magnetometry and scanning electron microscopy. These nanoparticles were applied for extraction and preconcentration of OPPs (residues of diazinon and fenitrothion, which are the most-widely used for pest control in Iran) in environmental water samples at low ng mL(-1) concentration as magnetic-SPE adsorbent. The extraction conditions and efficiency of the nanoparticles for OPPs were investigated. The method was evaluated according to the reproducibility, enrichment factor, linearity range and limits of detection. Under optimized conditions, method showed good linearity between 0.03-0.06 and 30 ng mL(-1) with regression coefficients (R(2)) of 0.997 and 0.998. Limits of detection were 0.019 and 0.014 ng mL(-1). The enrichment factors of this method were 172 and 184 and the analysis yielded good reproducibility with the RSD values 7.2% and 5.4% at the 10 ng mL(-1) level (n=5) for diazinon and fenitrothion, respectively. Determination of OPPs can be easily carried out with this fast, accurate, sensitive and simple method procedure.

  6. Preconcentration and determination of Sn- and Pb-organic species in environmental samples by SPME and GC-AED.

    PubMed

    Tutschku, S; Mothes, S; Wennrich, R

    1996-03-01

    A new sample preparation and preconcentration technique - solid phase microextraction (SPME) - is reported for the application of several tinorganic compounds and tetrabutyllead in aqueous samples. The solvent-free procedure is rapid in comparison with liquid-liquid extraction or SFE but also sensitive. Analytical variables of the extraction such as adsorption and desorption time, stirring rate and temperature has been investigated. The determination has been performed by GC coupled with atomic emission detection (AED). After optimization of the conditions of SPME a calibration was realized on the basis of a multicomponent standard solution, prepared by ethylation of organotin salts directly in the sample using sodium tetraethylborate (NaBEt(4)) without prior separation of the analytes from the matrix. The method permits preconcentration. Values of about 10 can be reached. A detection limit of 0.09 pg Sn and 0.08 pg Pb can be achieved under optimized conditions. The proposed procedure has been successfully applied to the analysis of organotin compounds in various slurry samples. PMID:15067450

  7. Determination of rare earth elements in natural water samples - A review of sample separation, preconcentration and direct methodologies.

    PubMed

    Fisher, Andrew; Kara, Derya

    2016-09-01

    This review discusses and compares the methods given for the determination of rare earth elements (REE) in natural water samples, including sea, river, lake, tap, ground and waste waters as well as Antarctic ice. Since REE are at very low concentrations in natural waters, numerous different preconcentration methods have been proposed to enable their measurement. These include liquid liquid extraction, dispersive liquid-liquid micro-extraction and solidified floating drop micro-extraction. In addition to liquid-liquid extraction methods, solid phase extraction using commercial resins, resins made in-house, silica-based exchange materials and other solid media is also discussed. These and other techniques such as precipitation/co-precipitation and flotation are compared in terms of speed, preconcentration factors achieved, precision, accuracy and limits of detection (LOD). Some papers have discussed the direct determination of REE in these sample types. Some have used specialised sample introduction systems such as ultrasonic nebulization whereas others have used a standard sample introduction system coupled with inductively coupled plasma mass spectrometry (ICP-MS) detection. These direct methods have also been discussed and compared.

  8. A new spectrophotometric method for determination of selenium in cosmetic and pharmaceutical preparations after preconcentration with cloud point extraction.

    PubMed

    Soruraddin, Mohammad Hosein; Heydari, Rouhollah; Puladvand, Morteza; Zahedi, Mir Mehdi

    2011-01-01

    A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV) was described. In this method, all selenium spices reduced to selenium (IV) using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV) in aqueous solution. The proposed method is based on the complexation of Selenium (IV) with dithizone at pH < 1 in micellar medium (Triton X-100). After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm) and dithizone (434 nm) overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL(-1); the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL(-1) of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples.

  9. Cloud point extraction-flame atomic absorption spectrometry method for preconcentration and determination of trace cadmium in water samples.

    PubMed

    Ning, Jinyan; Jiao, Yang; Zhao, Jiao; Meng, Lifen; Yang, Yaling

    2014-01-01

    A method based on cloud point extraction (CPE) separation/preconcentration of trace cadmium (Cd) as a prior step to its determination by flame atomic absorption spectrometry has been developed. Cadmium reacted with 8-hydroxyquinoline to form hydrophobic chelates, which were extracted into the micelles of nonionic surfactant oligoethylene glycol monoalkyl ether (Genapol X-080) in an alkaline medium. Octanol was used to depress the cloud point of Genapol X-080 in the extraction process. The chemical variables that affect the CPE, such as pH of complexation reaction, amount of chelating agent, Genapol X-080 and octanol were evaluated and optimized. Under optimized conditions, linearity was obeyed in the range of 10-500 μg/L, with the correlation coefficient of 0.9993. For 5 mL of sample solution, the enhancement factor was about 20. The limit of detection and limit of quantification of the method were 0.21 and 0.63 μg/L, respectively. The relative standard deviations (n = 6) was 3.2% for a solution containing 100 μg/L of Cd. The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. Recoveries of spiked samples varied in the range of 94.1-103.8%.

  10. Cloud-point extraction, preconcentration and spectrophotometric determination of trace quantities of copper in food, water and biological samples.

    PubMed

    Gouda, Ayman A; Amin, Alaa S

    2014-01-01

    A new, simple and sensitive cloud point extraction procedure was presented for the preconcentration and determination of copper(II) ion in food, water and biological samples. The analyte was complexed with a new synthesized reagent, 2-amino-4-(m-tolylazo)pyridine-3-ol (ATAP) as a new complexing agent and Triton X-114 as the surfactant. After centrifugation, dilution of the surfactant-rich phase with 0.4 mL of ethanol acidified with 1.0M HNO3 was performed after phase separation, and the copper contents were measured by spectrophotometry at λmax 608 nm. The influence of analytical parameters including concentration of complexing agent, Triton X-114, pH, equilibration temperature and time, centrifuge rate and time were optimized. The analytical characteristics of the method (e.g. linear range, molar absorptivity, Sandell sensitivity, optimum Ringbom concentration ranges limits of detection and quantification, preconcentration factor, and improvement factors) were obtained. Linearity was obeyed in the range of 4.0-115 ng mL(-1) of Cu(II) ion. The detection and quantification limits of the method were 1.20 and 3.94 ng mL(-1) of Cu(II) ion, respectively. The interference effect of some anions and cations was also tested. The method was applied for determination of copper in food, water and biological samples.

  11. Micro-flow injection analysis system: on-chip sample preconcentration, injection and delivery using coupled monolithic electroosmotic pumps.

    PubMed

    Nie, Fu-Qiang; Macka, Mirek; Paull, Brett

    2007-11-01

    A micro-fluidic chip, within which two monolithic electroosmotic pumps are utilised for sample preconcentration, injection and delivery is presented. The monolithic pumps were capable of producing stable and bubble free flow rates at applied voltages below 2 kV, with a current <10 microA. Electrokinetic (EK) sample injection, down to low nano-litre volumes, was quantitatively controlled through applied voltage and injection times, whilst the sample pump delivered a carrier solution to indirectly dispense the sample. A nano-flow sensor (NFS) was used to continuously monitor the flow rate stability of each pump, showing response times of <5-10 s for changes in applied voltage. A capacitively coupled contactless conductivity detector (C(4)D), as an off-chip on-capillary detector, was used to complete the micro-flow injection analysis (FIA) system. A monolithic electroosmotic pump (EOP), modified with an anionic surfactant, was used to demonstrate a novel approach to on-chip cation preconcentration and elution.

  12. CZE separation of amitrol and triazine herbicides in environmental water samples with acid-assisted on-column preconcentration.

    PubMed

    Arribas, Alberto Sánchez; Moreno, Mónica; Bermejo, Esperanza; Zapardiel, Antonio; Chicharro, Manuel

    2011-01-01

    A simple analytical scheme for the detection and quantification of amitrol and triazine herbicides (atrazine, ametryn and atraton) and degradation product (2-hydroxyatrazine) in environmental water samples by CZE is reported. On-column preconcentration of analytes from untreated water samples (mineral, spring, tap and river water) is accomplished by introducing an acid plug (200 mM citrate of pH 2.0) after the sample and then proceeding with the CZE separation, using 100 mM formiate buffer of pH 3.5 as running buffer and 25.0 KV as separation voltage. UV detection at 200 nm provides LODs from 50 to 300 nM in untreated samples and they were lowered tenfold by sample preconcentration by evaporation. Calculated recoveries were typically higher than 90%. Minimal detectable concentration of the electroactive amitrol could be decreased about 20-fold when electrochemical detection was employed by monitoring the amperometric signal at +800 mV using a carbon paste electrode (LOD of 9.6 nM, 0.81 μg/L, versus 170 nM, 14.3 μg/L, using amperometric and UV detection, respectively) in untreated water samples. PMID:21254126

  13. [Determination of mercury and copper in water samples by activation analysis using preconcentration on emission spectroscopic carbon powder (author's transl)].

    PubMed

    Nagatsuka, S; Tanizaki, Y

    1978-07-01

    A simple preconcentration procedure for mercury and copper was examined in the activation analysis of water samples. The preconcentration using pure activated carbon has been reported in several papers. The authors found that the carbon powder for emission spectroscopic analysis showed the high purity equivalent to pure activated carbon. The influence of various parameters in adsorption conditions was studied by radioactive tracers 197Hg and 64Cu. It was confirmed that 100% of these elements were adsorbed on carbon powders as pyrrolidine dithiocarbonate complexes at an acidity of pH 6--8, the temperature of 50 degrees C and the stirring time of 30 minutes. This method was applied to the activation analysis of the river water samples taken from the upper stream area of the Arakawa river and the ground water samples taken from the upper stream area of the Arakawa river and the ground water samples taken from the wells of the environs of Tokyo Megapolis. The carbon powders which adsorbed these elements were filtered, dried and analyzed by instrumental neutron activation analysis. The Hg concentrations of 0.01--0.1 ppb in river water and 0.03--1.4 ppb in ground water were obtained as well as the Cu concentrations of 0.3--3.0 ppb in ground water. The limits of determination of this method are 0.01 ppb Hg and 0.2 ppb Cu in the case of 11 sample of fresh water. PMID:704956

  14. Intelligent identification of wear mechanism via on-line ferrograph images

    NASA Astrophysics Data System (ADS)

    Wu, Tonghai; Peng, Yeping; Sheng, Chenxing; Wu, Jiaoyi

    2014-03-01

    Condition based maintenance(CBM) issues a new challenge of real-time monitoring for machine health maintenance. Wear state monitoring becomes the bottle-neck of CBM due to the lack of on-line information acquiring means. The wear mechanism judgment with characteristic wear debris has been widely adopted in off-line wear analysis; however, on-line wear mechanism characterization remains a big problem. In this paper, the wear mechanism identification via on-line ferrograph images is studied. To obtain isolated wear debris in an on-line ferrograph image, the deposition mechanism of wear debris in on-line ferrograph sensor is studied. The study result shows wear debris chain is the main morphology due to local magnetic field around the deposited wear debris. Accordingly, an improved sampling route for on-line wear debris deposition is designed with focus on the self-adjustment deposition time. As a result, isolated wear debris can be obtained in an on-line image, which facilitates the feature extraction of characteristic wear debris. By referring to the knowledge of analytical ferrograph, four dimensionless morphological features, including equivalent dimension, length-width ratio, shape factor, and contour fractal dimension of characteristic wear debris are extracted for distinguishing four typical wear mechanisms including normal, cutting, fatigue, and severe sliding wear. Furthermore, a feed-forward neural network is adopted to construct an automatic wear mechanism identification model. By training with the samples from analytical ferrograph, the model might identify some typical characteristic wear debris in an on-line ferrograph image. This paper performs a meaningful exploratory for on-line wear mechanism analysis, and the obtained results will provide a feasible way for on-line wear state monitoring.

  15. FEDIX on-line information service: Design, develop, test, and implement an on-line research and education information service. Annual status report, September 1992--August 1993

    SciTech Connect

    Rodman, J.A.

    1993-08-01

    Federal Information Exchange, Inc. (FIE) is a diversified information services company that is recognized as the major electronic link between the higher education community and the Federal government in the field of research administration. FIE provides a range of information related services to the government, academic and private sectors, including database management, software development and technical support. FEDIX is the on-line information service designed, developed and implemented by FIE to accomplish the following objectives: (1). Broaden the participation of the education community in Federal research and education programs by providing free and unrestricted on-line access to information from all participating Federal agencies; and (2). Provide the education community with on-line access to a single keyword-searchable system for research and educational funding opportunities at the participating Federal agencies.

  16. Assessment of trace aluminium content in parenteral solutions by combined cloud point preconcentration-flow injection inductively coupled plasma optical emission spectrometry.

    PubMed

    Sombra, Lorena L; Luconi, Marta O; Fernández, Liliana P; Olsina, Roberto A; Silva, María F; Martínez, Luis D

    2003-01-01

    A micelle-mediated phase separation without added chelating agents to preconcentrate trace levels of aluminium in parenteral solutions as a prior step to its determination by flow injection inductively coupled plasma optical emission spectrometry has been developed. The enrichment step is based on the cloud point extraction of aluminium with the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5). The chemical variables affecting the sensitivity of the extractive-spectrometric procedure were studied in detail. After optimization, a preconcentration factor of 200 and a %E higher than 99.9 were achieved. The detection limit (DL) value of aluminium for the preconcentration of 50 ml of parenteral solution was 0.25 microgl(-1). The calibration graph using the preconcentration system for aluminium was linear with a correlation coefficient of 0.9997 at levels near the DLs up to at least 200 microgl(-1). The developed hyphenated assay, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate to monitor the aluminium concentration in parenteral nutrition.

  17. Preconcentration of low levels of americium and plutonium from waste waters by synthetic water-soluble metal-binding polymers with ultrafiltration

    SciTech Connect

    Smith, B.F.; Gibson, R.R.; Jarvinen, G.D.; Robison, T.W.; Schroeder, N.C.; Stalnaker, N.D.

    1997-12-31

    A preconcentration approach to assist in the measurement of low levels of americium and plutonium in waste waters has been developed based on the concept of using water-soluble metal-binding polymers in combination with ultrafiltration. The method has been optimized to give over 90% recovery and accountability from actual waste water.

  18. A Micro-Preconcentrator Combined Olfactory Sensing System with a Micromechanical Cantilever Sensor for Detecting 2,4-Dinitrotoluene Gas Vapor.

    PubMed

    Chae, Myung-Sic; Kim, Jinsik; Yoo, Yong Kyoung; Kang, Ji Yoon; Lee, Jeong Hoon; Hwang, Kyo Seon

    2015-01-01

    Preventing unexpected explosive attacks and tracing explosion-related molecules require the development of highly sensitive gas-vapor detection systems. For that purpose, a micromechanical cantilever-based olfactory sensing system including a sample preconcentrator was developed to detect 2,4-dinitrotoluene (2,4-DNT), which is a well-known by-product of the explosive molecule trinitrotoluene (TNT) and exists in concentrations on the order of parts per billion in the atmosphere at room temperature. A peptide receptor (His-Pro-Asn-Phe-Ser-Lys-Tyr-Ile-Leu-His-Gln-Arg) that has high binding affinity for 2,4-DNT was immobilized on the surface of the cantilever sensors to detect 2,4-DNT vapor for highly selective detection. A micro-preconcentrator (µPC) was developed using Tenax-TA adsorbent to produce higher concentrations of 2,4-DNT molecules. The preconcentration was achieved via adsorption and thermal desorption phenomena occurring between target molecules and the adsorbent. The µPC directly integrated with a cantilever sensor and enhanced the sensitivity of the cantilever sensor as a pretreatment tool for the target vapor. The response was rapidly saturated within 5 min and sustained for more than 10 min when the concentrated vapor was introduced. By calculating preconcentration factor values, we verified that the cantilever sensor provides up to an eightfold improvement in sensing performance.

  19. The ASDC Multi Mission Interactive Archive: on line analysis of the Swift/XRT data

    SciTech Connect

    Stratta, G.; Capalbi, M.; Perri, M.; Giommi, P.

    2010-10-15

    We present the Swift/XRT Interactive Archive and the On-line Analysis tool developed at the ASI Science Data Center (ASDC) as part of the Multi Mission Interactive Archive. The On-line Analysis enables to run the Swift/XRT software task ''xrtpipeline'' on any desired XRT observation present in the Swift data archive maintained at ASDC, directly on the web. On-line imaging (with XIMAGE), spectral (with XSPEC) and timing data analysis (with LCURVE) can be performed. At the same time, spectra, light curves, effective area, exposure map and response matrix are promptly available for download to the user for any off-line analysis.

  20. Evaluation of performance of three different hybrid mesoporous solids based on silica for preconcentration purposes in analytical chemistry: From the study of sorption features to the determination of elements of group IB.

    PubMed

    Kim, Manuela Leticia; Tudino, Mabel Beatríz

    2010-08-15

    Several studies involving the physicochemical interaction of three silica based hybrid mesoporous materials with metal ions of the group IB have been performed in order to employ them for preconcentration purposes in the determination of traces of Cu(II), Ag(I) and Au(III). The three solids were obtained from mesoporous silica functionalized with 3-aminopropyl (APS), 3-mercaptopropyl (MPS) and N-[2-aminoethyl]-3-aminopropyl (NN) groups, respectively. Adsorption capacities for Au, Cu and Ag were calculated using Langmuir's isotherm model and then, the optimal values for the retention of each element onto each one of the solids were found. Physicochemical data obtained under thermodynamic equilibrium and under kinetic conditions - imposed by flow through experiments - allowed the design of simple analytical methodologies where the solids were employed as fillings of microcolumns held in continuous systems coupled on-line to an atomic absorption spectrometry. In order to control the interaction between the filling and the analyte at short times (flow through conditions) and thus, its effect on the analytical signal and the presence of interferences, the initial adsorption velocities were calculated using the pseudo second order model. All these experiments allowed the comparison of the solids in terms of their analytical behaviour at the moment of facing the determination of the three elements. Under optimized conditions mainly given by the features of the filling, the analytical methodologies developed in this work showed excellent performances with limits of detection of 0.14, 0.02 and 0.025 microg L(-1) and RSD % values of 3.4, 2.7 and 3.1 for Au, Cu and Ag, respectively. A full discussion of the main findings on the interaction metal ions/fillings will be provided. The analytical results for the determination of the three metals will be also presented.

  1. On-line in-syringe magnetic stirring assisted dispersive liquid-liquid microextraction HPLC--UV method for UV filters determination using 1-hexyl-3-methylimidazolium hexafluorophosphate as extractant.

    PubMed

    Suárez, Ruth; Clavijo, Sabrina; Avivar, Jessica; Cerdà, Víctor

    2016-02-01

    An environmental friendly and fully automated method using in-syringe magnetic stirring assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography has been developed for the determination of UV filters in environmental water samples. The main "green" features on this method are the use of an ionic liquid as extracting solvent, avoiding the use of chlorinated solvents, and the on-line microextraction, preconcentration, separation and detection minimizing the use of reagents and so the waste generation. After sample treatment, 20 µL of the organic droplet was injected onto the HPLC-UV system. Various parameters affecting the extraction efficiency were studied using multivariate optimization approach, including the quantity of extraction and dispersive solvents, extraction and sedimentation time, ionic strength and pH. Under optimized conditions, limits of detection were within the range of 0.08-12 µg/L, for 3.5 mL sample volume. Linearity ranges were up to 500 µg/L for the UV-filters studied. Furthermore, enrichment factors ranging from 11 to 23 folds were obtained. Intra- and inter-assay precisions were 6% and 8%, respectively. Finally, the proposed method was successfully applied to determine UV filters in surface seawater and swimming pool samples attaining satisfactory recoveries over the range of 89-114% and 86-107%, respectively. PMID:26653488

  2. Synthesis and application of a new functionalized resin for use in an on-line, solid phase extraction system for the determination of trace elements in waters and reference cereal materials by flame atomic absorption spectrometry.

    PubMed

    Karadaş, Cennet; Turhan, Onur; Kara, Derya

    2013-11-15

    The synthesis and characterization of the resin Amberlite XAD-4 functionalized with 2,6-pyridinedicarboxaldehyde and its application in an on-line system for the preconcentration of cadmium, cobalt, copper, lead and manganese prior to determination using flame atomic absorption spectrometry (FAAS) is proposed. Metal ions retained on the modified resin were eluted using 1.0 mol L(-1) HNO3 solution and aspirated directly to the nebulizer-burner system of a FAAS instrument using a flow injection system. Detection limits (3σ) were determined to be 0.13 μg L(-1) for Cd, 0.29 μg L(-1) for Cu, 0.23 μg L(-1) for Mn, 0.58 μg L(-1) for Co and 2.19 μg L(-1) for Pb using a 10 mL of water sample loading volume. The limits of detection would be 100 times higher with units of μg kg(-1) for the solid samples in which their dilution ratios as (volume/weight) were 100. Enrichment factors ranged from 23.6 to 28.9 (for Co and Mn, respectively). The proposed method was successfully applied to determination of the analytes in natural water samples and certified reference materials.

  3. Synthesis and application of a new functionalized resin for use in an on-line, solid phase extraction system for the determination of trace elements in waters and reference cereal materials by flame atomic absorption spectrometry.

    PubMed

    Karadaş, Cennet; Turhan, Onur; Kara, Derya

    2013-11-15

    The synthesis and characterization of the resin Amberlite XAD-4 functionalized with 2,6-pyridinedicarboxaldehyde and its application in an on-line system for the preconcentration of cadmium, cobalt, copper, lead and manganese prior to determination using flame atomic absorption spectrometry (FAAS) is proposed. Metal ions retained on the modified resin were eluted using 1.0 mol L(-1) HNO3 solution and aspirated directly to the nebulizer-burner system of a FAAS instrument using a flow injection system. Detection limits (3σ) were determined to be 0.13 μg L(-1) for Cd, 0.29 μg L(-1) for Cu, 0.23 μg L(-1) for Mn, 0.58 μg L(-1) for Co and 2.19 μg L(-1) for Pb using a 10 mL of water sample loading volume. The limits of detection would be 100 times higher with units of μg kg(-1) for the solid samples in which their dilution ratios as (volume/weight) were 100. Enrichment factors ranged from 23.6 to 28.9 (for Co and Mn, respectively). The proposed method was successfully applied to determination of the analytes in natural water samples and certified reference materials. PMID:23790831

  4. On-line monitoring of mercury and hydrogen chloride in hot gases from coal gasifiers

    SciTech Connect

    Norton, G.A.; Chriswell, C.D.; Eckels, D.E.; Buttermore, W.H.

    1993-09-01

    A variety of analytical techniques which may be applicable to monitoring Hg or HCl in METC gasifier streams were identified. Potential approaches for on-line analysis of Hg and HCl are discussed in detail.

  5. Integration of On-Line and Off-Line Diagnostic Algorithms for Aircraft Engine Health Management

    NASA Technical Reports Server (NTRS)

    Kobayashi, Takahisa; Simon, Donald L.

    2007-01-01

    This paper investigates the integration of on-line and off-line diagnostic algorithms for aircraft gas turbine engines. The on-line diagnostic algorithm is designed for in-flight fault detection. It continuously monitors engine outputs for anomalous signatures induced by faults. The off-line diagnostic algorithm is designed to track engine health degradation over the lifetime of an engine. It estimates engine health degradation periodically over the course of the engine s life. The estimate generated by the off-line algorithm is used to update the on-line algorithm. Through this integration, the on-line algorithm becomes aware of engine health degradation, and its effectiveness to detect faults can be maintained while the engine continues to degrade. The benefit of this integration is investigated in a simulation environment using a nonlinear engine model.

  6. On-Line Serials Control System in a Large Biomedical Library: (1) Description of the System

    ERIC Educational Resources Information Center

    Fayollat, James

    1972-01-01

    An on-line serials control system with particular emphasis on storage and maintenance concepts is described. The system allows real-time display and updating of all elements of the file. (6 references) (Author)

  7. Quantitative high-resolution on-line NMR spectroscopy in reaction and process monitoring

    NASA Astrophysics Data System (ADS)

    Maiwald, Michael; Fischer, Holger H.; Kim, Young-Kyu; Albert, Klaus; Hasse, Hans

    2004-02-01

    On-line nuclear magnetic resonance spectroscopy (on-line NMR) is a powerful technique for reaction and process monitoring. Different set-ups for direct coupling of reaction and separation equipment with on-line NMR spectroscopy are described. NMR spectroscopy can be used to obtain both qualitative and quantitative information from complex reacting multicomponent mixtures for equilibrium or reaction kinetic studies. Commercial NMR probes can be used at pressures up to 35 MPa and temperatures up to 400 K. Applications are presented for studies of equilibria and kinetics of complex formaldehyde-containing mixtures as well as homogeneously and heterogeneously catalyzed esterification kinetics. Direct coupling of a thin-film evaporator is described as an example for the benefits of on-line NMR spectroscopy in process monitoring.

  8. ON-LINE TOOLS FOR PROPER VERTICAL POSITIONING OF VERTICAL SAMPLING INTERVALS DURING SITE ASSESSMENT

    EPA Science Inventory

    This presentation presents on-line tools for proper vertical positioning of vertical sampling intervals during site assessment. Proper vertical sample interval selection is critical for generate data on the vertical distribution of contamination. Without vertical delineation, th...

  9. On line high dose static position monitoring by ionization chamber detector for industrial gamma irradiators.

    PubMed

    Rodrigues, Ary A; Vieira, Jose M; Hamada, Margarida M

    2010-01-01

    A 1 cm(3) cylindrical ionization chamber was developed to measure high doses on line during the sample irradiation in static position, in a (60)Co industrial plant. The developed ionization chamber showed to be suitable for use as a dosimeter on line. A good linearity of the detector was found between the dose and the accumulated charge, independently of the different dose rates caused by absorbing materials.

  10. First structures on RyantoRainbow Line. Hframe structure on Line 1 ...

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

    First structures on Ryan-to-Rainbow Line. H-frame structure on Line 1 (right) has historic porcelain suspension insulators and H-frame structure on Line 2 (center) has two historic porcelain insulators and one modern non-ceramic insulator. View to north - Ryan Hydroelectric Facility, Ryan-to-Rainbow 100 kV Transmission Line, West bank of Missouri River, northeast of Great Falls, Great Falls, Cascade County, MT

  11. Column chromatographic preconcentration of copper in alloys and complex materials using 9,10 phenanthrenequinone monoxime supported on naphthalene

    SciTech Connect

    Puri, B.K.; Balani, S. )

    1992-03-01

    A solid chelating compound phenanthrenequinone monoxime (PQM) supported on naphthalene provides a rapid and economical means of preconcentration and separation of copper from the aqueous samples. Copper forms a complex with PQM supported on naphthalene in the column at pH 6.1-8.4 with a flow rate of 1 ml/min. The metal complex and naphthalene are dissolved out from the column with 5 ml of DMP and the absorbance is measured at 470 nm against reagent blank. Beer's law is obeyed in the concentration range 0.6-9.6 {mu}g of copper in 5 ml of DMF. The molar absorptivity and sensitivity are 6.3 {times} 10{sup 4} L mol{sup {minus} 1} cm{sup {minus} 1} and 0.001 {mu}g cm{sup {minus} 2} respectively.

  12. Novel modified carbon nanotubes as a selective sorbent for preconcentration and determination of trace copper ions in fruit samples.

    PubMed

    Rezvani, Mehdi; Ebrahimzadeh, Homeira; Aliakbari, Azam; Khalilzadeh, Azita; Kasaeian, Mansoure; Amini, Mostafa M

    2014-09-01

    In this work, multiwalled carbon nanotubes were reacted with N-[3-(triet-hoxysilyl)propyl]isonicotinamide to prepare pyridine-functionalized carbon nanotubes. This novel sorbent was characterized by infrared spectroscopy, thermal and elemental analysis, and scanning electron microscopy. Functionalized carbon nanotubes were applied for the preconcentration and determination of copper ions using flame atomic absorption spectrometry. Various parameters such as sample pH, flow rate, eluent type and concentration, and its volume were optimized. Under optimal experimental conditions, the limit of detection, the relative standard deviation, and the recovery of the method were 0.65 ng/mL, 3.2% and 99.4%, respectively. After validating the method using standard reference materials, the new sorbent was applied for the extraction and determination of trace copper(II) ions in fruit samples.

  13. Spectrophotometric determination of trace sulphate in rain and snow after preconcentration with 2-aminoperimidine on a membrane filter.

    PubMed

    Shida, J; Satake, H; Ono, N; Fujikura, T

    1990-06-01

    A simple and precise preconcentration technique, based on collecting a precipitate on a membrane filter and dissolving the filter and precipitate in an organic solvent, has been applied to the spectrophotometric determination of trace sulphate in rain and snow. The sulphate is precipitated with 2-aminoperimidine and the resulting compound is dissolved in nitric acid, made alkaline with sodium hydroxide and then adsorbed on tetradecyldimethylbenzylammonium nitrate. The precipitate is then collected on a membrane filter and both precipitate and filter are dissolved in dimethylsulphoxide (DMSO). The absorbance of the DMSO solution is measured at 550 nm against a reagent blank. The molar absorptivity is 2.1 x 10(4) 1 . mole(-1) . cm(-1) and the coefficient of variation for six measurements is < 1.5%. The detection limit (S/N = 3) is 0.06 mug of sulphate in 5 ml of sample solution.

  14. Ionic liquids for simultaneous preconcentration of some lanthanoids using dispersive liquid-liquid microextraction technique in uranium dioxide powder.

    PubMed

    Mallah, Mohammad H; Shemirani, Farzaneh; Maragheh, Mohammad G

    2009-03-15

    Ionic liquids in a dispersive liquid-liquid microextraction technique were used for determination of lanthanoids such as samarium, europium, gadolinium, and dysprosium in uranium dioxide powder. In this process, an appropriate mixture of extraction solvent and disperser is rapidly injected into an aqueous sample containing samarium, europium, gadolinium, and dysprosium ions complexes with 1-hydroxy-2, 5-pyrrolidinedione, and consequently a cloudy solution is formed. It consists of fine droplets of extraction solventwhich are dispersed entirely into the aqueous phase. After centrifugation of this solution, the whole enriched phase was determined by inductively coupled plasma optical emission spectrometry. In the present work, the preconcentration factor, limit of detection, and relative standard deviation were investigated for samarium, europium, gadolinium, and dysprosium in uranium dioxide powder. PMID:19368197

  15. Cloud point extraction-atomic absorption spectrometry for pre-concentration and determination of cadmium in cigarette samples.

    PubMed

    Tavallali, Hossein; Boustani, Fazlollah; Yazdandoust, Mozhdeh; Aalaei, Mehdi; Tabandeh, Mahboobeh

    2013-05-01

    A new complexing agent, 2-((2-((1H-benzo[d]imidazole-2yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazole (BIMPI), was used in cloud point extraction and applied for selective pre-concentration of trace amounts of cadmium in cigarette samples. Cadmium was complexed with BIMPI in a buffer solution (pH = 10) using Triton X-114 as surfactant and quantitatively extracted into a small volume of the surfactant-rich phase after centrifugation. Under optimized conditions (pH = 10.0, 0.8 × 10(-4) mol L(-1) BIMPI and 0.08 % (w/v) Triton X-114), calibration graph was linear in the range of 34.0-1,670.0 μg L(-1). The proposed method was applied to the determination of Cd in various cigarette (tobacco) samples which gave satisfactory results.

  16. Analysis of trace metals in water by inductively coupled plasma emission spectrometry using sodium dibenzyldithiocarbamate for preconcentration

    USGS Publications Warehouse

    Smith, C.L.; Motooka, J.M.; Willson, W.R.

    1984-01-01

    Since concentrations of trace elements in most natural waters seldom exceed the ??g/L level, analysis of trace elements in natural waters by inductively coupled plasma emission spectrometry (ICP) requires a preconcentration procedure. The elements Ag, Bi, Cd, Co, Cu, Fe, Mo, Ni, Pb, Sn, V, W, and Zn were separated and concentrated from 500 mL of water by coprecipitating them with sodium dibenzyldithiocarbamate (NaDBDTC) using nickel or silver as a carrier. The precipitated trace elements were collected on a membrane filter, redissolved from the filter with hot nitric and hydrochloric acids, and analyzed using ICP. Recoveries for all the trace elements except tungsten exceeded 80%. Coprecipitation of trace elements with NaDBDTC eliminated the use of difficult-to-inject organic solvents, and NaDBDTC coprecipitated a wider array of trace elements than ammoniumpyrrolidinedithiocarbamate (APDC), another commonly used coprecipitate.

  17. A new coprecipitation methodology with lutetium hydroxide for preconcentration of heavy metal ions in herbal plant samples.

    PubMed

    Soylak, Mustafa; Murat, Ipek

    2014-01-01

    A new coprecipitation methodology that used lutetium hydroxide as a precipitant for Cu(II), Pb(II), Mn(II), Co(II), Cd(II), Fe(III), and Ni(II) ions in herbal plant and water samples for analysis by atomic absorption spectrometry has been investigated. The parameters such as pH, amount of lutetium, and volume of aqueous sample were optimized for the recovery of these seven metals. The effects of concomitant ions on the separation-preconcentration of analytes were also checked. The validation of the procedure was checked with addition recovery tests and analysis of Standard Reference Material 1570a-Trace Elements in Spinach Leaves and TMDA-70 fortified lake water Certified Reference Material. The LODs for analyte ions were in the range of 1.7-7.2 microg/L. The application of the present procedure was successfully performed for the analysis of analyte contents of herbal plant samples from Turkey.

  18. Hydrophobic polydimethylsiloxane (PDMS) coating of mesoporous silica and its use as a preconcentrating agent of gas analytes.

    PubMed

    Park, Eun Ji; Cho, Youn Kyoung; Kim, Dae Han; Jeong, Myung-Geun; Kim, Yong Ho; Kim, Young Dok

    2014-09-01

    Mesoporous silica with mean pore size of ∼14 nm was coated by polydimethylsiloxane (PDMS) using a thermal deposition method. We showed that the inner walls of pores larger than ∼8 nm can be coated by thin layers of PDMS, and the surfaces consisting of PDMS-coated silica were superhydrophobic, with water contact angles close to 170°. We used the PDMS-coated silica as adsorbents of various gas-phase chemical warfare agent (CWA) simulants. PDMS-coated silica allowed molecular desorption of various CWA simulants even after exposure under highly humid conditions and, therefore, is applicable as an agent for the preconcentration of gas-phase analytes to enhance the sensitivities of various sensors. PMID:25102134

  19. On-Line Wavelength Calibration of Pulsed Laser for CO2 Differential Absorption LIDAR

    NASA Astrophysics Data System (ADS)

    Xiang, Chengzhi; Ma, Xin; Han, Ge; Liang, Ailin; Gong, Wei

    2016-06-01

    Differential absorption lidar (DIAL) remote sensing is a promising technology for atmospheric CO2 detection. However, stringent wavelength accuracy and stability are required in DIAL system. Accurate on-line wavelength calibration is a crucial procedure for retrieving atmospheric CO2 concentration using the DIAL, particularly when pulsed lasers are adopted in the system. Large fluctuations in the intensities of a pulsed laser pose a great challenge for accurate on-line wavelength calibration. In this paper, a wavelength calibration strategy based on multi-wavelength scanning (MWS) was proposed for accurate on-line wavelength calibration of a pulsed laser for CO2 detection. The MWS conducted segmented sampling across the CO2 absorption line with appropriate number of points and range of widths by using a tunable laser. Complete absorption line of CO2 can be obtained through a curve fitting. Then, the on-line wavelength can be easily found at the peak of the absorption line. Furthermore, another algorithm called the energy matching was introduced in the MWS to eliminate the backlash error of tunable lasers during the process of on-line wavelength calibration. Finally, a series of tests was conducted to elevate the calibration precision of MWS. Analysis of tests demonstrated that the MWS proposed in this paper could calibrate the on-line wavelength of pulsed laser accurately and steadily.

  20. The synthesis of new polymeric sorbent and its application in preconcentration of cadmium and lead in water samples.

    PubMed

    Senkal, B Filiz; Ince, Muharrem; Yavuz, Erdem; Yaman, Mehmet

    2007-05-15

    Metal determinations at low concentration levels (preconcentration techniques still continues increasingly for trace metal determinations by flame atomic absorption spectrometry (FAAS) due to the high accuracy of this method. In this work, thioureasulfonamide resin was synthesized, characterized and applied as a new sorption material for determinations of cadmium and lead in water samples. The method is based on the sorption of Cd and Pb ions on the synthesized resin without using any complexing reagent. The optimization of experimental conditions was performed using factorial design including pH, amount of resin, contact time, first sample volume and final eluent volume. Using the experimental conditions defined in the optimization, the method was applied to the determination and preconcentration of Cd and Pb at ngmL(-1) level in natural water. Flame AAS was used for trace metal determinations. This method exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent and optimum pH of solution presents in acidic media. Consequently, 600- and 360-fold improvements in the sensitivity of FAAS were achieved by combining the slotted tube atom trap-atomic absorption spectrometry (STAT-FAAS) and the purposed enrichment method for Cd and Pb, respectively.