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Sample records for on-line bead-injection preconcentration

  1. Hyphenating multisyringe flow injection lab-on-valve analysis with atomic fluorescence spectrometry for on-line bead injection preconcentration and determination of trace levels of hydride-forming elements in environmental samples.

    PubMed

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald; Estela, José Manuel; Cerdà, Víctor

    2006-12-15

    In this work the third generation of flow injection analysis, that is, the so-called micro-lab-on-valve (microLOV) approach, is proposed for the first time for the separation, preconcentration, and monitoring of metalloids as hyphenated with atomic fluorescence spectrometry (AFS). This was made feasible by interfacing the micromachined LOV-module with AFS by a multisyringe flowing stream network for on-line postcolumn derivatization of the eluate aimed at generation of hydride species. The potential of this new hyphenated technique for environmental assays was ascertained via determination of ultratrace level concentrations of total inorganic arsenic in freshwater. Employing quantitative preoxidation of As(III) to As(V) in the samples by means of permanganate, the method involves preconcentration of arsenate at pH 10 on a renewable anion exchanger, namely, Q-Sepharose, packed in a LOV microcolumn. The analyte species is afterward stripped out and concurrently prereduced by a 300 microL eluent plug containing 6 mol L(-)1 HCl and 10% KI. The eluate is downstream merged with a metered volume of sodium tetrahydroborate (0.3% w/v) for generation of arsine, which is subsequently quantified by AFS. The flow system facilitates on-column reduction of the retained arsenic with no need for application of programmable stopped flow. Yet, the high concentration of reductant and extreme pH conditions for elution hinder the sorbent to be reused due to gradual deactivation of the functional moieties, so that maximum benefit can be taken from the application of the bead renewable strategy. The proposed procedure is characterized by a high tolerance to metal species and interfering hydride-forming elements. In fact, ratios of Se(IV) to As < or = 5000 and Sb(V) to As < or = 500 are tolerated at the 10% interference level. Under the optimized experimental conditions, a detection limit (3sigma) of 0.02 ng mL(-1) As, a dynamic linear range of 0.05-2.0 ng mL(-1) As (by tailoring the AFS

  2. 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

  3. Recent applications of on-line sample preconcentration techniques in capillary electrophoresis.

    PubMed

    Kitagawa, Fumihiko; Otsuka, Koji

    2014-03-28

    This review highlights recent developments and applications of on-line sample preconcentration techniques in capillary electrophoresis (CE) from 2010 to April 2013. Various preconcentration techniques based on the analyte velocity change in two or three discontinuous solutions system including field-amplified stacking, transient isotachophoresis, pH-mediated stacking, sweeping, and their modified and combined techniques have been employed to enrich and separate biological, environmental, food, toxicological, forensic and nanoparticle samples in CE. More than 170 published research articles collected from Scopus databases from the year 2010 described the on-line sample preconcentration techniques. This review provides comprehensive tables listing the applications of the on-line sample preconcentration techniques with categorizing by the fundamental preconcentration mechanism and application area. PMID:24210300

  4. Strategies for the on-line preconcentration and separation of hypolipidaemic drugs using micellar electrokinetic chromatography.

    PubMed

    Dawod, Mohamed; Breadmore, Michael C; Guijt, Rosanne M; Haddad, Paul R

    2010-01-15

    Three strategies were investigated for the simultaneous separation and on-line preconcentration of charged and neutral hypolipidaemic drugs in micellar electrokinetic chromatography (MEKC). A background electrolyte (BGE) consisting of 20 mM ammonium bicarbonate buffer (pH 8.50) and 50 mM sodium dodecyl sulfate (SDS) was used for the separation and on-line preconcentration of the drugs. The efficiencies of sweeping, analyte focusing by micelle collapse (AFMC), and simultaneous field-amplified sample stacking (FASS) and sweeping, were compared for the preconcentration of eight hypolipidaemic drugs in different conductivity sample matrices. When compared with a hydrodynamic injection (5 s at 50 mbar, 0.51% of capillary volume to detection window) of drug mixture prepared in the separation BGE, improvements of detection sensitivity of 60-, 83-, and 80-fold were obtained with sweeping, AFMC and simultaneous FASS and sweeping, respectively, giving limits of detection (LODs) of 50, 36, and 38 microg/L, respectively. The studied techniques showed suitability for focusing different types of analytes having different values of retention factor (k). This is the first report for the separation of different types of hypolipidaemic drugs by capillary electrophoresis (CE). The three methods were validated then applied for the analysis of target analytes in wastewater samples from Hobart city. PMID:20015504

  5. 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

  6. Application of polyurethane foam loaded with BTAC in an on-line preconcentration system: cadmium determination by FAAS

    NASA Astrophysics Data System (ADS)

    Lemos, Valfredo A.; Santelli, Ricardo E.; de Carvalho, Marcelo S.; Ferreira, Sérgio L. C.

    2000-09-01

    In the present paper, the use of polyurethane foam modified by 2-(2-benzothiazolylazo)-2- p-cresol (BTAC) as a sorbent in an on-line preconcentration system to determine cadmium trace levels by FAAS is proposed. The procedure was based on the chemical sorption of cadmium (II) ions onto a minicolumn packed with polyurethane foam, followed by 0.10 mol l -1 hydrochloric acid elution and direct determination by Flame Atomic Absorption Spectrometry. The flow system was operated in a time-based mode. Chemical and flow variables were studied. Results demonstrated that sample solutions containing cadmium(II) in the range of concentration from 0.91 to 30.00 μg l -1, pH between 6.50 and 9.25 could be determinated by this procedure, in a preconcentration time of 1 min. Flow rates in preconcentration and elution steps were 7.00 and 4.00 ml min -1, respectively. The precision of the preconcentration procedure (evaluated as standard deviation of solutions containing 1.0-30.0 μg l -1 of cadmium) varied in the range from 5 to 1%. The preconcentration factor, calculated as the ratio of the linear section of the slopes of the analytical curves before and after preconcentration, was 41, for a volume sample of 7.00 ml. The detection limit was 0.27 μg l -1 for a preconcentration time of 1 min. The proposed procedure was applied for determination of cadmium in biological reference materials. Achieved results demonstrated that the procedure can be applied for analysis of biological materials with satisfactory accuracy.

  7. 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

  8. 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

  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. On-line Determination of Zinc in Water and Biological Samples after Its Preconcentration onto Zincon Anchored Polyurethane Foam.

    PubMed

    Azeem, Sami M Abdel; Hanafi, Hassan A; El-Shahat, M F

    2015-01-01

    A fast and sensitive on-line procedure for the determination of zinc in water and biological samples was developed. Zinc was preconcentrated in a mini-column packed with polyurethane foam (PUF) chemically modified with zincon via -N=N- bonding. The optimal conditions for preconcentration were pH 8.5 and sample flow rate of 4.0 mL min(-1). Quantitative desorption of Zn(II) was obtained by 0.1 mol L(-1) hydrochloric acid and subsequent spectrophotmetric determination using 4-(2-pyridylazo)-resorcinol at 498 nm. The obtained detection limit was found to be 3.0 ng mL(-1), precision (RSD) was 4.8 and 6.7% at 20 and 110 ng mL(-1), respectively, for 60 s preconcentration time and enrichment factor was 31. The linearity range was from 10 to 120 ng mL(-1) and maximum sample throughput was 20 h(-1). Finally, the method was successfully applied to the determination of zinc in tap water, Nile River water and human urine samples with RSD in the range of 1.1 - 8.3%. PMID:25958868

  11. 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

  12. On-line preconcentration and determination of lead and cadmium by sequential injection/anodic stripping voltammetry.

    PubMed

    Ninwong, Benjawan; Chuanuwatanakul, Suchada; Chailapakul, Orawon; Dungchai, Wijitar; Motomizu, Shoji

    2012-07-15

    The highly sensitive determination of lead (Pb(II)) and cadmium (Cd(II)) ions, with a limit of detection of 0.01μgL(-1) for Pb(II) and Cd(II), by on-line preconcentration and anodic stripping voltammetry (ASV) controlled by a sequential injection analysis (SIA) system is reported here. The SIA system consisted of a syringe pump, an 8-port selection valve and a 6-port switching valve and was incorporated with a bismuth coated screen-printed carbon nanotube electrode (Bi-SPCNTE). The preconcentration of metal ions was performed by solid phase extraction using an Analig TE-05 chelating resin mini-column on a switching valve. The metal ions collected were then eluted from the resin with 1M hydrochloric acid (HCl), deposited on the electrode surface at -1.3V vs. Ag/AgCl and then measured with ASV. The pH of the sample, eluent volume, flow rate, concentration of the bismuth plating solution and the square-wave voltammetric parameters were optimized. Under the optimum conditions, an enrichment factor of 11.9-fold and 6.6-fold for Pb(II) and Cd(II) ions, respectively, was attained. Detection of Pb(II) and Cd(II) had two different linear ranges (0.5-15μgL(-1) and 15-70μgL(-1)). PMID:22817931

  13. 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. PMID:17822233

  14. 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

  15. An optimized procedure for preconcentration, determination and on-line recovery of palladium using highly selective diphenyldiketone-monothiosemicarbazone modified silica gel.

    PubMed

    Sharma, R K; Pandey, Amit; Gulati, Shikha; Adholeya, Alok

    2012-03-30

    A novel, highly selective, efficient and reusable chelating resin, diphenyldiketone-monothiosemicarbazone modified silica gel, was prepared and applied for the on-line separation and preconcentration of Pd(II) ions in catalytic converter and spiked tap water samples. Several parameters like effect of pH, sample volume, flow rate, type of eluent, and influence of various ionic interferences, etc. were evaluated for effective adsorption of palladium at trace levels. The resin was found to be highly selective for Pd(II) ions in the pH range 4-5 with a very high sorption capacity of 0.73 mmol/g and preconcentration factor of 335. The present environment friendly procedure has also been applied for large-scale extraction by employing the use of newly designed reactor in which on-line separation and preconcentration of Pd can be carried out easily and efficiently in short duration of time. PMID:22296710

  16. 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

  17. 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...

  18. 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

  19. 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

  20. [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%. PMID:22295800

  1. 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

  2. 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.

  3. On-line preconcentration/determination of lead in Ilex paraguariensis samples (mate tea) using polyurethane foam as filter and USN-ICP-OES.

    PubMed

    Marchisio, P F; Sales, A; Cerutti, S; Marchevski, E; Martinez, L D

    2005-09-30

    The present paper proposes an on-line preconcentration procedure for lead determination in Ilex paraguariensis (St. Hilaire) samples by ultrasonic nebulization associated to inductively coupled plasma optical emission spectrometry (USN-ICP-OES). It is based on the precipitation of lead(II) ion on a minicolumn packed with polyurethane foam using 2-(5-bromo-2-pyridilazo)-5-diethylaminophenol (5-Br-PADAP) as precipitating reagent. The collected analyte precipitate was quantitatively eluted from the minicolumn with 20% (v/v) nitric acid. An enhancement factor of 225-fold was obtained (15 for USN and 15 for preconcentration). The detection limit (DL) value for the preconcentration of 10.0 ml of sample was 40.0 ng/l. The relative standard deviation (R.S.D.) was 3.0% for a Pb concentration of 1 microg/l, calculated from the peak heights obtained. The calibration graph using the preconcentration system for lead was linear with a correlation coefficient of 0.9997, at levels near the detection limits up to at least 100 microg/l. The preconcentration procedure was successfully applied to the determination of lead in mate tea samples. PMID:15936141

  4. 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. PMID:25637009

  5. 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

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

    PubMed

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

    2015-09-01

    A new on-line SPE-HPLC method using fused-core columns for on-line solid phase extraction and large volume sample injection for increasing the sensitivity of detection was developed for the determination of insecticides fenoxycarb and cis-, trans-permethrin in surface waters. The separation was carried out on fused-core column Phenyl-Hexyl (100×4.6 mm), particle size 2.7 µm with mobile phase acetonitrile:water in gradient mode at flow rate 1.0 mL min(-1), column temperature 45°C. Large volume sample injection (1500 µL) to the extraction dimension using short precolumn Ascentis Express RP C-18 (5×4.6 mm); fused-core particle size 2.7 µm allowed effective sample preconcentration and efficient ballast sample matrix removal. The washing mobile phase consisting of a mixture of acetonitrile:water; 30:70, (v/v) was pumped at flow rate of 0.5 mL min(-1) through the extraction precolumn to the waste. Time of the valve switch for transferring the preconcentrated sample zone from the extraction to the separation column was set at 3rd min. Elution of preconcentrated insecticides from the extraction precolumn and separation on the analytical column was performed in gradient mode. Linear gradient elution started from 40% of acetonitrile at time of valve switch from SPE column (3rd min) to 95% of acetonitrile at 7th min. Synthetic dye sudan I was chosen as an internal standard. UV detection at wavelength 225 nm was used and the method reached the limits of detection (LOD) at ng mL(-1) levels for both insecticides. The method showing on-line sample pretreatment and preconcentration with highly sensitive determination of insecticides was applied for monitoring of fenoxycarb and both permethrin isomers in different surface water samples in Czech Republic. The time of whole analysis including on-line extraction, interferences removal, chromatography separation and system equilibration was less than 8 min. PMID:26003701

  7. Factorial design for multivariate optimization of an on-line preconcentration system for platinum determination by ultrasonic nebulization coupled to inductively coupled plasma optical emission spectrometry.

    PubMed

    Cerutti, S; Salonia, J A; Ferreira, S L C; Olsina, R A; Martinez, L D

    2004-07-01

    A system for on-line preconcentration and determination of platinum by ultrasonic nebulization (USN) coupled to inductively coupled plasma optical emission spectrometry (ICP-OES) was studied. It is based on the chemical sorption of platinum on a column packed with polyurethane foam loaded with thiocyanate reagent. The optimization step was carried out using two level full factorial design. Three variables (pH, loading flow rate (LFR) and eluent concentration) were regarded as factors in the optimization. Results of the two level factorial design 2(3) with three replicates of the central point for platinum preconcentration, based on the variance analysis (ANOVA), demonstrated that the factors and their interactions are not statistically significant. The proposed procedure allowed the determination of platinum with a detection limit of 0.28mugl(-1). The precision for 10 replicate determinations at 10.0mugl(-1) Pt level was 3.8% relative standard deviation (R.S.D.), calculated from the peak heights obtained. A total enhancement factor of 100 was obtained with respect to ICP-OES using pneumatic nebulization (10 for USN and 10 for preconcentration). A sampling frequency of 50 samples per hour was obtained. The effect of other ions in concentrations agreeing with water samples was studied. The addition/recovery experiments in the samples analyzed demonstrated the accuracy and applicability of the system developed for platinum determination in spiked water samples. PMID:18969536

  8. Trace determination of tetracyclines in water samples by capillary zone electrophoresis combining off-line and on-line sample preconcentration.

    PubMed

    Moreno-González, David; Lupión-Enríquez, Isabel; García-Campaña, Ana M

    2016-05-01

    In this work, a sensitive and reliable method using capillary zone electrophoresis with UV detection has been developed for trace determination of tetracycline antibiotics in river, spring, and ground waters. A solid-phase extraction method using Oasis HLB was applied for off-line preconcentration and cleanup of water samples, in combination with an on-line preconcentration methodology named large volume sample stacking with polarity switching. Different parameters were optimized in order to obtain an adequate separation combined with the highest sensitivity, using 75 mM sodium carbonate (pH 10) and 1 mM EDTA as separation buffer, applying a voltage of 25 kV at 25°C. The samples were injected in water at 1 bar for 1 min, applying then -25 kV and starting the sample stacking. Sample matrix removal from the capillary was controlled by monitoring the electric current (when the 95% of the separation current is reached the stacking process is completed). The applied voltage was then switched from negative to a positive value of 25 kV in order to separate the compounds. Under optimum conditions, sensitivity enhancement factors ranged from 303 to 428 for the studied compounds. The combination of both off-line and on-line preconcentration procedures provided a total sensitivity enhancement factor about 20 000, obtaining detection limits from 67 to 167 ng/L. The precision (intra- and interday), expressed as %RSD was below 12%. Recoveries obtained from river, spring, and ground waters ranged from 87 to 96%. Thus, this procedure is suitable for monitoring these compounds in water samples. PMID:27135309

  9. 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.

  10. On-line preconcentration of sodium dodecyl sulfate-protein complexes using electrokinetic supercharging method with a prefilled water plug in capillary sieving electrophoresis.

    PubMed

    Liu, Jing; Kang, Mingchao; Liu, Zhen

    2011-09-01

    An electrokinetic supercharging (EKS) method with a prefilled water plug at the head column of capillary was developed for on-line preconcentration of sodium dodecyl sulfate (SDS)-protein complexes in capillary sieving electrophoresis (CSE). Conventional EKS is a combination of electrokinetic injection with transient isotachophoresis (tr-ITP). The capillary is first filled with background electrolyte, then an appropriate amount of a leading electrolyte is filled and electro-injection is carried out for certain duration. After that, terminating electrolyte is filled, and tr-ITP is subsequently initiated, followed by capillary electrophoresis (CE) separation. In this work, the performance of EKS was evaluated by integrating multiple sub-methods step by step, and a water plug containing polymer was introduced before electrokinetic injection in order to further improve the concentration effect. The positive effects of the sub-methods were verified, including molecular sieving effect of polymer, field enhanced sample injection (FESI) with and without a water plug, and transient isotachophoretic electrophoresis-based FESI. It was observed that analyte discrimination usually encountered in conventional electrokinetic injection was eliminated due to the similar charge to mass ratios of SDS-protein complexes. Based on these results, a hybrid on-line preconcentration method, EKS with injecting a water plug containing polymer before sample electrokinetic injection, was proposed and used to indiscriminately preconcentrate SDS-protein complexes, which provided a sensitivity enhancement factor of more than 1000. It was very suitable for the analysis of low-abundance proteins, providing the information of their molecular mass. PMID:22233073

  11. 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

  12. On-line ion-exchange preconcentration and determination of traces of platinum by electrothermal atomic absorption spectrometry.

    PubMed

    González García, M M; Sánchez Rojas, F; Bosch Ojeda, C; García de Torres, A; Cano Pavón, J M

    2003-04-01

    A method to determine trace amounts of platinum in different samples based on electrothermal atomic absorption spectrometry is described. The preconcentration step is performed on a chelating resin microcolumn [1,5-bis(2-pyridyl)-3-sulfophenyl methylene thiocarbonohydrazide (PSTH) immobilized on an anion-exchange resin (Dowex 1x8-200)] placed in the autosampler arm. The combination of a peristaltic pump for sample loading and the atomic absorption spectrometer pumps for elution through a selection valve simplifies the hardware. The peristaltic pump and the selection valve are easily controlled electronically with two switches placed in the autosampler, which are activated when the autosampler arm is down. Thus, the process is fully automated without any modification of the software of the atomic absorption spectrometer. Under the optimum conditions with a 60-s preconcentration time, a sample flow rate of 2.4 mL min(-1), and an injection volume of eluent of 40 microL, a linear calibration graph was obtained in the range 0-100 ng mL(-1). The enrichment factor was 14. The detection limit under these conditions is 1 ng mL(-1), and the relative standard deviation (RSD) is 1.6% for 10 ng mL(-1) of Pt. The method has been applied to the determination of platinum in catalyst, vegetation, soil, and natural water samples. The results showed good agreement with the certified value and the recoveries of Pt added to samples were 98-105%. PMID:12733043

  13. 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

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

    PubMed

    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

  15. Electrokinetic supercharging for on-line preconcentration of seven non-steroidal anti-inflammatory drugs in water samples.

    PubMed

    Dawod, Mohamed; Breadmore, Michael C; Guijt, Rosanne M; Haddad, Paul R

    2008-05-01

    The development of new sensitive methods for the analysis of non-steroidal anti-inflammatory drugs (NSAIDs) in water samples is of great importance. In this work, seven NSAIDs were separated within 9 min using 15 mM sodium tetraborate (pH 9.2) containing 0.1% (w/v) hexadimethrine bromide (HDMB) and 10% (v/v) methanol. Field-amplified sample injection (FASI) was examined and found to improve the detection limits by 200-fold providing detection limits of 0.6-2.0 microg/L, but these are insufficient for the determination of NSAIDs as environmental pollutants in water samples. To improve the sensitivity further, electrokinetic supercharging (EKS) was examined. The optimum EKS method involved hydrodynamic injection leading electrolyte (100 mM NaCl, 30 s, 50 mbar), electrokinetic injection of the sample (200 s, -10 kV) and finally injection of the terminating electrolyte (100 mM 2-(cyclohexylamino) ethanesulphonic acid, CHES, 40s, 50 mbar). With this method, the sensitivity was improved by 2400-fold giving detection limits of 50-180 ng/L. The developed method was validated and then applied to the analysis of wastewater samples from a local sewage treatment plant. The detection limits were found to increase by approximately 10-fold, however, this is still lower than levels previously found in wastewater samples from European and Mediterranean cities. The proposed method has the advantage of simplicity and achieving sensitivity through high-preconcentration power without the use of off-line chromatographic sample cleanup. PMID:18206157

  16. Electrokinetic supercharging-electrospray ionisation-mass spectrometry for separation and on-line preconcentration of hypolipidaemic drugs in water samples.

    PubMed

    Dawod, Mohamed; Breadmore, Michael C; Guijt, Rosanne M; Haddad, Paul R

    2010-04-01

    Electrokinetic supercharging, a powerful on-line preconcentration technique in CE, was for the first time hyphenated with ESI-MS for the on-line concentration and separation of five hypolipidaemic drugs. The electrophoretic separation was performed in a co-EOF mode using the EOF reversal agent, hexadimethrine bromide, in ammonium bicarbonate electrolyte, pH 9.00. The ionic strength and the amount of methanol in the buffer were optimised in a multivariate manner using artificial neural networks, with the optimal conditions being 60 mM ammonium bicarbonate containing 60% methanol, providing baseline resolution of the five hypolipidaemics within 20 min. Using electrokinetic supercharging, the sensitivity of the method was improved 1000-fold over a conventional injection under field-amplified sample stacking conditions with LODs of 180 ng/L. This is the first report of the separation of hypolipidaemics by CE. The developed method was validated and then applied to the determination of the target drugs in water samples from Hobart city. PMID:20349512

  17. 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

  18. Multielement trace determinations in A1 2O 3 ceramic powders by inductively coupled plasma mass spectrometry with special reference to on-line trace preconcentration

    NASA Astrophysics Data System (ADS)

    Pollmann, D.; Leis, F.; Tölg, G.; Tschöpel, P.; Broekaert, J. A. C.

    1994-12-01

    The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of trace elements in Al 2O 3 powders is reported. Special interest is given to a preconcentration of the trace elements by on-line coupling of chromatography to ICP-MS. This is based on the complexation of Co, Cu, Cr, Fe, Ga, Mn, Ni, V and Zn with hexamethylene-dithiocarbamate (HMDC), their preconcentration on a C18 RP column by reversed phase liquid chromatography and their elution with CH 3OH-H 2O mixtures. A direct coupling of the HPLC system to the ICP-MS has been realized by high pressure pneumatic nebulization using desolvation. With the Chromatographie method developed, removal of the AI by at least 99% was achieved. For the trace elements V, Fe, Ni, Co, Cu and Ga, high and reproducible recoveries (ranging from 96-99%) were reached. The method developed has been shown to considerably enhance the power of detection as compared with direct procedures, namely down to 0.02-0.16 ( μg/g for V and Fe, respectively. The possibilities of the method are shown by the determinations of V, Mn, Fe, Ni, Co, Cu, Zn and Ga at the μg/g level in A1 2O 3 powders. The accuracy of the method at the 0.06 to 9.0 μg/g level for Co and Fe, respectively, is demonstrated by a comparison with results of independent methods from the literature.

  19. Fast speciation of mercury in seawater by short-column high-performance liquid chromatography hyphenated to inductively coupled plasma spectrometry after on-line cation exchange column preconcentration.

    PubMed

    Jia, Xiao-Yu; Gong, Di-Rong; Han, Yi; Wei, Chao; Duan, Tai-Cheng; Chen, Hang-Ting

    2012-01-15

    A simple and fast method for trace speciation analysis of mercury (Hg(2+)), methylmercury (MeHg(+)) and ethylmercury (EtHg(+)) in seawater has been developed by short-column high-performance liquid chromatography hyphenated to inductively coupled plasma spectrometry (HPLC-ICP-MS) after on-line cation-exchange column (CEC) preconcentration. The analytes were firstly adsorbed on the CEC without any extraneous reagent, and then were eluted rapidly (within seconds) and completely with a very low concentration of l-cysteine solution, which provides the conveniency for the on-line coupling of the preconcentration method and detection technique. To our best knowledge, it is for the first time to employ the CEC preconcentration technique to trap all of the three mercury species simultaneously at their positive charged status for the purpose of speciation analysis. Under the optimized conditions, a very high preconcentration factor up to 1250 has been obtained with 30mL sample solution, which leads to the very low detection limits of 0.042ngL(-1) for Hg(2+), 0.016ngL(-1) for MeHg(+) and 0.008ngL(-1) for EtHg(+) (as Hg), respectively. With the established method, three seawater samples were also analyzed, and all the three mercury species have been found in each sample, albeit at a very low concentration. PMID:22265565

  20. 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). PMID:18261513

  1. 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. PMID:12012188

  2. Gallium trace on-line preconcentration/separation and determination using a polyurethane foam mini-column and flame atomic absorption spectrometry. Application in aluminum alloys, natural waters and urine.

    PubMed

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

    2003-07-27

    A sensitive and selective flow injection time-based method for on-line preconcentration/separation and determination of gallium by flame atomic absorption spectrometry at trace levels was developed. The on-line formed gallium chloride complex is sorbed onto a polyether-type polyurethane foam mini-column, followed by on-line quantitative elution with isobutyl methyl ketone and direct introduction into the flame pneumatic nebulizer of the atomic absorption spectrometer. All chemical and flow variables of the system as well as the possible interferences were studied. The manner of strong HCl solutions propulsion was investigated and established using a combination of two displacement bottles. For 90 s preconcentration time, a sample frequency of 28 h(-1), an enhancement factor of 40, a detection limit of 6 microg l(-1) and a precision expressed as relative standard deviation (s(r)) of 3.3% (at 1.00 mg l(-1)) were achieved. The calibration curve is linear over the concentration range 0.02-3.00 mg l(-1). The accuracy of the developed method was sufficient and evaluated by the analysis of a silicon-aluminum alloy standard reference material. Finally, it was successfully applied to gallium determination in commercial aluminum alloys, natural waters and urine. PMID:18969117

  3. 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).

  4. 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. PMID:24274293

  5. On-line Ultrasound-Assisted Dispersive Micro-Solid-Phase Extraction Based on Amino Bimodal Mesoporous Silica Nanoparticles for the Preconcentration and Determination of Cadmium in Human Biological Samples.

    PubMed

    Shirkhanloo, H; Falahnejad, M; Zavvar Mousavi, H

    2016-06-01

    On-line ultrasound-assisted dispersive micro-solid-phase extraction (USA-DμSPE) has been developed for preconcentration and separation of trace amounts of Cd(II) ions in 0.5 mL of human biological samples. In a syringe with a nylon membrane, new synthetic bulky amino bimodal mesoporous silica nanoparticles (NH2-UVM7) were dispersed as a nanoadsorbent in 5 mL of diluted serum sample (1:10), and after ultrasonic shaking, the liquid phase was separated from the solid phase. At the optimized pH, the chemical and physical adsorption of cadmium ions occurred, respectively, based on complexation with amine groups of UVM7 (Cd:NH2-UVM7) and silica nanoparticles. The analyte was then back-extracted from the sorbent with nitric acid solution (0.2 M), and its concentration was determined by electrothermal atomic absorption spectrometry (ETAAS). Under the optimized conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were obtained as 0.01-0.56 μg L(-1), 0.002 μg L(-1), and 25, respectively. The adsorption capacity of NH2-UVM7 was found to be 108.6 mg g(-1) of cadmium. The validation of the methodology was performed by the human standard reference material (HSRM). PMID:26475301

  6. 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

  7. Hybrid mesoporous materials for on-line preconcentration of Cr(VI) followed by one-step scheme for elution and colorimetric determination at ultratrace levels.

    PubMed

    Kim, Manuela L; Stripeikis, Jorge D; Tudino, Mabel B

    2009-01-15

    An hybrid mesoporous material synthesised in our laboratories for solid phase extraction (SPE) in flow through systems has been used for analytical purposes. The solid was obtained from mesoporous silica MCM-41 functionalized with 3-aminopropyltriethoxy silane by Sol-Gel methodology. In order to exploit the large sorption capacity of the material together with the possibility of modeling it for anions retention, a microcolumn (MC) filled with the solid was inserted in a flow system for preconcentration of Cr(VI) and its determination at ultratrace levels in natural waters. The analytical methodology involved a reverse flow injection system (rFI) holding a MC filled with the solid for the analyte extraction. Elution and colorimetric detection were carried out with 1-5 diphenylcarbazide (DPC) in sulfuric acid. DPC produced the reduction of Cr(VI) to Cr(III) together with the generation of a cationic red complex between Cr(III) and 1-5 diphenylcarbazone which was easily eluted and detected with a visible spectrophotometer. Moreover, the filling material got ready for the next sample loading remaining unspoiled for more than 300 cycles. The effect of several variables on the analytical signal as well as the influence of cationic and anionic interferences were discussed. Particular attention was given to sulfuric acid interference since it is the required media for the complex generation. Under optimal conditions, 99.8% of Cr(VI) recovery was obtained for a preconcentration time of 120s (sample and DPC flow rates=1 mL min(-1)) and an elution volume of 250 micro L. The limit of detection (3s) was found to be 0.09 microg L(-1) Cr(VI) with a relative standard deviation (n=10, 3 microg L(-1)) of 1.8. Since no Cr(III) was retained by the solid material and Cr(VI) was completely adsorbed, electrothermal atomic absorption spectrometry (ET AAS) determinations of Cr(III) were also performed by simply measuring its concentration at the end of the microcolumn after Cr

  8. Immobilization of proteins on agarose beads, monitored in real time by bead injection spectroscopy

    PubMed Central

    Ruzicka*, Jaromir; Carroll, Andrea D.; Lähdesmäki, Ilkka

    2006-01-01

    Summary This work introduces a novel tool for the examination and optimization of protein immobilization protocols, by measuring the rate and yield of coupling reactions, as they take place on the surface of agarose beads in a well-stirred microreactor. The power of the Bead Injection Spectroscopy (BIS) technique is demonstrated on examples of amino coupling reactions for albumin, ovalbumin, lysozyme, human IgG, ribonuclease A and cytochrome C, using commercially available Aminolink® agarose beads. It was found, surprisingly, that currently recommended protocols for reductive amination can be shortened from several hours to several minutes, and that, contrary to literature data, the yield of coupling is dependent on pH and the isoelectric point of the protein. In addition, leakage of immobilized ligands can be measured by direct spectroscopic interrogation of captured beads in situ. The methodology presented in this work documents that BIS is a useful tool for quality control of agarose-based chromatographic supports, as well as for the optimization of a wide variety of immobilization chemistries, as used for synthesis of chromatographic supports, immobilization of enzymes, and derivatization of biosensing surfaces. PMID:16802025

  9. 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

  10. 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.

  11. 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. PMID:21557471

  12. 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.

  13. 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.

  14. Particle preconcentrator

    SciTech Connect

    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.

  15. Particle preconcentrator

    SciTech Connect

    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.

  16. Particle preconcentrator

    SciTech Connect

    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.

  17. 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").

  18. Exploiting the bead injection LOV approach to carry out spectrophotometric assays in wine: application to the determination of iron.

    PubMed

    Vidigal, Susana S M P; Tóth, Ildikó V; Rangel, António O S S

    2011-06-15

    A sequential injection lab-on-valve (SI-LOV) system was used to develop a new methodology for the determination of iron in wine samples exploiting the bead injection (BI) concept for solid phase extraction and spectrophotometric measurement. Nitrilotriacetic Acid (NTA) Superflow resin was used to build the bead column of the flow through sensor. The iron (III) ions were retained by the bead column and react with SCN(-) producing an intense red colour. The change in absorbance was monitored spectrophotometrically on the optosensor at 480 nm. It was possible to achieve a linear range of 0.09-5.0 mg L(-1) of iron, with low sample and reagent consumption; 500 μL of sample, 15 μmol of SCN(-), and 9 μmol of H(2)O(2), per assay. The proposed method was successfully applied to the determination of iron in wine, with no previous treatment other than dilution, and to other food samples. PMID:21641441

  19. 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.

  20. 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.

  1. 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

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. [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

  7. 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.

  8. 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

  9. 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.

  10. Preconcentration modeling for the optimization of a micro gas preconcentrator applied to environmental monitoring.

    PubMed

    Camara, Malick; Breuil, Philippe; Briand, Danick; Viricelle, Jean-Paul; Pijolat, Christophe; de Rooij, Nico F

    2015-04-21

    This paper presents the optimization of a micro gas preconcentrator (μ-GP) system applied to atmospheric pollution monitoring, with the help of a complete modeling of the preconcentration cycle. Two different approaches based on kinetic equations are used to illustrate the behavior of the micro gas preconcentrator for given experimental conditions. The need for high adsorption flow and heating rate and for low desorption flow and detection volume is demonstrated in this paper. Preliminary to this optimization, the preconcentration factor is discussed and a definition is proposed. PMID:25810264

  11. 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.

  12. Evaluation of adsorption preconcentration/capillary zone electrophoresis/nanoelectrospray mass spectrometry for peptide and glycoprotein analyses.

    PubMed

    Bateman, K P; White, R L; Thibault, P

    1998-11-01

    The use of an on-line adsorption preconcentrator coupled with capillary zone electrophoresis/nanoelectrospray mass spectrometry (PC/CZE/nESMS) is described for the analysis of peptides and protein digests. The investigation was focused on the production of disposable preconcentrators made of large particle size (40 microns irregular packing), thereby eliminating the use of a retaining frit without loss of performance. These preconcentration devices were made of commercially available components which can be easily interfaced to current CZE/nESMS systems. Practical issues such as the composition of the stationary phase, the elution volume and sample breakthrough and carry-over were evaluated in order to optimize the analytical performance of this technique. Under optimized elution conditions, the PC/CZE/nESMS technique provided separation efficiencies in excess of 100,000 theoretical plates for a sample loading of 8 microliters. Sample carry-over was minimized by proper reconditioning of the preconcentrator prior to the CZE separation. Alternatively, the sample carry-over resulting from small elution volumes could be used advantageously to provide multiple analyses from a single injection of sample. The application of this technique is demonstrated for the analysis of proteolytic peptides from a Bauhinia purpurea lectin at a concentration level of 30 nM. Further structural information was obtained using on-line tandem mass spectrometry to elucidate the structure of N-linked glycans and the amino acid sequences of the glycopeptides. PMID:9835067

  13. 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.

  14. CLOSED CYCLE COOLER FOR VOC PRECONCENTRATION

    EPA Science Inventory

    The objective of this study was to evaluate a reduced-temperature preconcentrator to replace pr reduce liquid cryogen use in field applications of automated gas chromatographs. he cooler was to be evaluated as a refocusing unit downstream of a solid sorbent trap. losed cycle cool...

  15. PRECONCENTRATION METHODS FOR TRACE ELEMENT DETERMINATION

    EPA Science Inventory

    This research had several objectives. One was to review the literature to determine methods of trace element preconcentration that could be used realistically for sample preparation for trace element determinations in drinking, natural and/or effluent waters. Elements included in...

  16. 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

  17. Preconcentration and separation of analytes in microchannels

    DOEpatents

    Hatch, Anson; Singh, Anup K.; Herr, Amy E.; Throckmorton, Daniel J.

    2010-11-09

    Disclosed herein are methods and devices for preconcentrating and separating analytes such as proteins and polynucleotides in microchannels. As disclosed, at least one size-exclusion polymeric element is adjacent to processing area or an assay area in a microchannel which may be porous polymeric element. The size-exclusion polymeric element may be used to manipulate, e.g. concentrate, analytes in a sample prior to assaying in the assay area.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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…

  3. Nanofluidic preconcentration and detection of nanoparticles

    NASA Astrophysics Data System (ADS)

    Mitra, Anirban; Ignatovich, Filipp; Novotny, Lukas

    2012-07-01

    The fast detection and characterization of nanoparticles, such as viruses or environmental pollutants, are important in fields ranging from biosensing to quality control. However, most existing techniques have practical throughput limitations, which significantly limit their applicability to low analyte concentrations. Here, we present an integrated nanofluidic scheme for preconcentration and subsequent detection of nanoparticle samples within a continuous flow-through system. Using a Brownian ratchet mechanism, we increase the nanoparticle concentration ˜27-fold. Single nanoparticles are subsequently detected and characterized by optical heterodyne interferometry. A wide range of potential applications can be foreseen, including real-time analysis of clinically relevant virus samples and contamination control of processing fluids used in the semiconductor industry.

  4. 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.

  5. 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.

  6. High-throughput liquid-absorption preconcentrator sampling methods

    DOEpatents

    Zaromb, S.

    1994-07-12

    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.

  7. 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.

  8. Preconcentration procedures for phthalate esters combined with chromatographic analysis.

    PubMed

    Lv, Xueju; Hao, Yi; Jia, Qiong

    2013-08-01

    Phthalate esters are endocrine disrupters or mutagens. They are widely used as plasticizers and can be usually found in environmental samples, such as food, soil and polluted air. However, it is difficult to directly determine phthalate esters owing to their relatively low concentration and complex matrices. Therefore, preconcentration and separation have become increasingly important. In recent years, many preconcentration methods have been successfully developed and widely used, such as liquid-liquid extraction, dispersive liquid-liquid microextraction and solid-phase extraction. These preconcentration methods for phthalate esters can be applied to various real samples, water, soil, air, food and cosmetics. The aim of this paper is to review recent literature studies (primarily from the last five years) about preconcentration techniques for phthalate esters coupled with chromatographic analysis. The following text describes several preconcentration approaches, including liquid-liquid extraction, dispersive liquid-liquid microextraction, cloud point extraction, solid-phase extraction, solid-phase microextraction and stir bar sorptive extraction. Their advantages and disadvantages are also summarized. PMID:23696389

  9. 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.

  10. 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.

  11. Sterility Testing by Capillary Electrophoresis: A Comparison of On-line Preconcentration Approaches in Capillaries with Greater Internal Diameters

    PubMed Central

    Petr, Jan; Jiang, Chunxia; Sevcik, Juraj; Tesarova, Eva; Armstrong, Daniel W.

    2015-01-01

    Detection of microbial contamination is of critical importance in the medical and the food industry. Rapid tests for the absence or presence of viable microorganisms are in urgent demand. Capillary electrophoresis is a modern analytical technique that can be adapted for rapid screening of microbial contamination. However, the small dimensions of capillaries allow introduction of only a small fraction of the sample, which can be problematic when examining large samples. In this article, we examine the possibilities of introducing larger sample volumes using capillaries with greater internal diameters (i.d.) together with different stacking techniques. The use of 0.32 mm i.d. capillary and the injection of 60 % of the capillary volume led to approximately 120-fold improvement of the injected sample volume over the classical injection 5% of a 0.10 mm i.d. capillary. The setup we described opens new possibilities in sterility testing using capillary electrophoresis. PMID:19847804

  12. 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...

  13. 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.

  14. 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.

  15. 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.

  16. 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 ...

  17. 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.

  18. On-line solid phase extraction with polyurethane foam: trace level spectrophotometric determination of iron in natural waters and biological materials.

    PubMed

    Cassella, Ricardo J

    2002-08-01

    This paper reports the development of a simple and accurate on-line procedure for preconcentration and determination of dissolved iron in waters and biological materials using unloaded polyether-type polyurethane foam as solid extractor. In the developed flow injection system, the analyte was preconcentrated from acidic aqueous medium as iron-thiocyanate complex with post-elution with ascorbic acid solution and spectrophotometric measurement with 1,10-phenanthroline as colorimetric reagent. In order to improve the performance of the system several chemical and flow variables were investigated as well as the effect caused by the presence of possible interferents. The method was validated by the analysis of two certified reference materials. Application of the methodology was carried out by the determination of dissolved iron content in eight natural water samples with different characteristics. The results were compared with those obtained by electrothermal atomic absorption spectrometry (ETAAS) and no statistical difference was observed. The detection limit was 0.75 microgram l-1 and the RSD was 1.2% for 2 min preconcentration time. At this condition, a productivity of 20 samples h-1 was achieved. Increasing the preconcentration time up to 3 min, a detection limit of 0.45 microgram l-1, an RSD of 1.5% and an analytical throughput of 15 h-1 were verified. PMID:12195994

  19. 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)

  20. 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…

  1. On-line diagnosis of sequential systems

    NASA Technical Reports Server (NTRS)

    Sundstrom, R. J.

    1973-01-01

    A model for on-line diagnosis was investigated for discrete-time systems, and resettable sequential systems. Generalized notions of a realization are discussed along with fault tolerance and errors. Further investigation into the theory of on-line diagnosis is recommended for three levels: binary state-assigned level, logical circuit level, and the subsystem-network level.

  2. 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

  3. 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.

  4. Trace metal preconcentration using a thioglycolate chelating resin

    SciTech Connect

    Howard, A.G.; Danilona-Mirzaians, R.

    1989-01-01

    A styrene-divinyl benzene copolymer resin (Amberlite XAD-4), modified with thioglycolate complexing groups, has been employed for the preconcentration of cadmium, zinc, lead and nickel from natural waters. The resin exhibits its strongest affinity for cadmium and lead but can be used to quantitatively remove all four metals from non-saline waters. With seawater samples, the resin is best only employed for the enrichment of cadmium and lead as the recovery of nickel and zinc from this medium is poor.

  5. Infrared micro-thermography of an actively heated preconcentrator device

    NASA Astrophysics Data System (ADS)

    Furstenberg, Robert; Kendziora, C. A.; Stepnowski, Stanley V.; Mott, David R.; McGill, R. Andrew

    2008-03-01

    We report infrared micro-thermography measurements and analysis of static and transient temperature maps of an actively heated micro-fabricated preconcentrator device that incorporates a dual serpentine platinum heater trace deposited on a perforated polyimide membrane and suspended over a silicon frame. The sorbent coated perforated membrane is used to collect vapors and gases that flow through the preconcentrator. After heating, a concentrated pulse of analyte is released into the detector. Due to its small thermal mass, precise thermal management of the preconcentrator is critical to its performance. The sizes of features, the semi-transparent membrane, the need to flow air through the device, and changes in surface emissivity on a micron scale present many challenges for traditional infrared micro-thermography. We report an improved experimental test-bed. The hardware incorporates a custom-designed miniature calibration oven which, in conjunction with spatial filtering and a simple calibration algorithm, allows accurate temperature maps to be obtained. The test-bed incorporates a micro-bolometer array as the infrared imager. Instrumentation design, calibration and image processing algorithms are discussed and analyzed. The procedure does not require prior knowledge of the emissivity. We show that relatively inexpensive uncooled bolometers arrays can be used in certain radiometric applications. Heating profiles were examined with both uniform and non-uniform air flow through the device. The conclusions from this study provide critical information for optimal integration of the preconcentrator within a detection system, and in the design of the heater trace layout to achieve a more even temperature distribution across the device.

  6. 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

  7. 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.

  8. On-line measurement of perchlorate in atmospheric aerosol based on ion chromatograph coupled with particle collector and post-column concentrator.

    PubMed

    Takeuchi, Masaki; Yoshioka, Kaoru; Toyama, Yusuke; Kagami, Ai; Tanaka, Hideji

    2012-08-15

    An automated analysis system has been developed for measuring perchlorate concentration in atmospheric aerosol. The perchlorate in aerosol sample, which has been collected with water mist in a hydrophobic filter/mist chamber based particle collector, is continuously preconcentrated. The matrix ions such as sulfate are subsequently removed from the preconcentrator. The remaining perchlorate is then analyzed on-line with an ion chromatograph in conjunction with a Nafion membrane tube based post-column concentrator. The sensitivity is increased by a factor of 7.7 with the post-column concentration technique. The proposed system has been successfully operated at Tokushima, Japan. The limit of detection is 0.35 ng/m(3) for 3 h sampling cycle. The perchlorate concentration in the atmospheric aerosol averaged 1.01±1.75 ng/m(3) (n=12). PMID:22841118

  9. On-line chemical composition analyzer development

    SciTech Connect

    Garrison, A.A.

    1993-01-01

    This report relates to the development of an on-line Raman analyzer for control of a distillation column. It is divided into: program issues, experimental control system evaluation, energy savings analysis, and reliability analysis. (DLC)

  10. On-Line Measurement of Aphasic Speech.

    ERIC Educational Resources Information Center

    Packman, Ann; Ingham, Roger J.

    1978-01-01

    The spontaneous speech of five aphasic Ss (47-70 years old) was rated on-line by four clinicians to test the reliability of seven response categories (devised for the concurrent evaluation of aphasic speech). (Author/PHR)

  11. 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

  12. On-line handwritten text categorization

    NASA Astrophysics Data System (ADS)

    Peña Saldarriaga, Sebastián; Viard-Gaudin, Christian; Morin, Emmanuel

    2009-01-01

    As new innovative devices, accepting or producing on-line documents, emerge, managing facilities for these kinds of documents such as topic spotting are required. This means that we should be able to perform text categorization of on-line documents. The textual data available in on-line documents can be extracted through online recognition, a process which produces noise, i.e. errors, in the resulting text. This work reports experiments on categorization of on-line handwritten documents based on their textual contents. We analyze the effect of the word recognition rate on the categorization performances, by comparing the performances of a categorization system over the texts obtained through on-line handwriting recognition and the same texts available as ground truth. Two categorization algorithms (kNN and SVM) are compared in this work. A subset of the Reuters-21578 corpus consisting of more than 2000 handwritten documents has been collected for this study. Results show that accuracy loss is not significant, and precision loss is only significant for recall values of 60%-80% depending on the noise levels.

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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

  20. Reflections of an On-Line Tutor

    ERIC Educational Resources Information Center

    Towndrow, Phillip

    2004-01-01

    This article investigates the relatively unexplored field of reflective journal writing by an on-line tutor, in this case working with a group of Chinese learners of English attending an intensive communication skills programme at a tertiary-level institution in Singapore. The results reported highlight the role of the reflective journal in…

  1. Student System, On-Line Admissions.

    ERIC Educational Resources Information Center

    White, Stephen R.

    This report provides technical information on an on-line admissions system developed by Montgomery College. Part I, Systems Development, describes the background, objectives and responsibilities, system design, and reports generated by the system. Part II, Operating Instructions, describes input forms and controls, admission system functions, file…

  2. Student System, On-Line Registration.

    ERIC Educational Resources Information Center

    Michael, Mary Ellen

    This report provides technical information on an on-line student registration system developed by Montgomery College. Part I, Systems Development, describes the background, objectives and benefits, system design, and reports generated by the system. Part II, Operating Instructions, describes input forms, registration system functions, file…

  3. 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...

  4. Transformation invariant on-line target recognition.

    PubMed

    Iftekharuddin, Khan M

    2011-06-01

    Transformation invariant automatic target recognition (ATR) has been an active research area due to its widespread applications in defense, robotics, medical imaging and geographic scene analysis. The primary goal for this paper is to obtain an on-line ATR system for targets in presence of image transformations, such as rotation, translation, scale and occlusion as well as resolution changes. We investigate biologically inspired adaptive critic design (ACD) neural network (NN) models for on-line learning of such transformations. We further exploit reinforcement learning (RL) in ACD framework to obtain transformation invariant ATR. We exploit two ACD designs, such as heuristic dynamic programming (HDP) and dual heuristic dynamic programming (DHP) to obtain transformation invariant ATR. We obtain extensive statistical evaluations of proposed on-line ATR networks using both simulated image transformations and real benchmark facial image database, UMIST, with pose variations. Our simulations show promising results for learning transformations in simulated images and authenticating out-of plane rotated face images. Comparing the two on-line ATR designs, HDP outperforms DHP in learning capability and robustness and is more tolerant to noise. The computational time involved in HDP is also less than that of DHP. On the other hand, DHP achieves a 100% success rate more frequently than HDP for individual targets, and the residual critic error in DHP is generally smaller than that of HDP. Mathematical analyses of both our RL-based on-line ATR designs are also obtained to provide a sufficient condition for asymptotic convergence in a statistical average sense. PMID:21571610

  5. 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.

  6. On-line handwriting analysis using wavelets

    NASA Astrophysics Data System (ADS)

    Srikantan, Geetha; Srihari, Rohini K.

    1995-09-01

    Speech and Handwriting interfaces to computing devices have received increased attention recently as alternate human-computer media. Automatic recognition of unconstrained handwritten text must be provided as a capability in handwriting computer interfaces. Variation in writing styles of a single writer at different times and between multiple writers makes unconstrained on-line handwriting recognition a challenging task. On-line handwriting is recorded as a sequence of coordinates as the writer's pen moves along the recording device. Isolated character and word recognition have been addressed by several researchers. More recently, attention has been focussed on the recognition of unconstrained text streams. The dynamic changes in handwriting styles observed in everyday use requires development of methods that are adaptive to local variations. We present a novel application of wavelet-based analysis of pen position, velocity and acceleration time-sequences for segmentation and recognition of text components.

  7. 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.

  8. The EINSTEIN On-Line Service

    NASA Astrophysics Data System (ADS)

    Harris, D. E.; Grant, C. S.; Andernach, H.

    The Einstein On-Line Service (EOLS) is a simple menu-driven system which provides an intuitive method of querying over one hundred database catalogs. In addition, the EOLS contains over 30 CD-ROMs of images from the Einstein X-ray Observatory which are available for downloading. The EOLS provides all of our databases to the NASA Astrophysics Data System (ADS) and our documents which describe each table are written in the ADS format. In conjunction with the IAU working group on Radioastronomical Databases, the EOLS serves as an experimental platform for on-line access to radio source catalogs. The number of entries in these catalogs exceeds half a million.

  9. 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

  10. Patient monitoring: on-line computing

    PubMed Central

    Raison, John C. A.

    1970-01-01

    On-line computing represents a further extension of the senses of attendant staff in intensive care situations. Smaller computers will contribute as scientific processors, by extending the capability of instrumental systems or enabling new means of measurement and calculation. The fullest use of computer-aid will provide systems of data acquisition from multiple sources, rapid processing correlation, analysis in mathematical and diagnostic forms, and resultant output in simply intelligible displays: later, some direct control of therapy may be applied. PMID:5476133

  11. Connecting to On-line Data

    NASA Astrophysics Data System (ADS)

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

    2004-05-01

    The Astrophysics Datacenter Executive Committee (ADEC) is coordinating the development of a system to facilitate the linking to on-line data. This system has three components: 1. Unique dataset identifiers. 2. A verification system for identifiers. 3. Permanent links to on-line data sets. 1. The ADEC has agreed on a naming scheme for data sets that allows for the unique identification of any data set. The ADEC data centers will clearly mark their data with these identifiers to allow the generation of links to these data. 2. Each data center has a utility that can check whether a data set identifier is a valid identifier at that center. A central verifier allows third parties access to these individual verifiers through a single portal. 3. The central verifier also provides permanent links to data sets through a central link forwarding system. This makes it possible to move data sets between data centers while maintaining the permanent links. The ADEC plans to first use this system to implement the linking from the literature to on-line data in a collaboration with the AAS and the University of Chicago Press for the AAS journals.

  12. On-line diagnosis of unrestricted faults

    NASA Technical Reports Server (NTRS)

    Meyer, J. F.; Sundstrom, R. J.

    1974-01-01

    A formal model for the study of on-line diagnosis is introduced and used to investigate the diagnosis of unrestricted faults. A fault of a system S is considered to be a transformation of S into another system S' 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' thereafter. Notions of fault tolerance error are defined in terms of the resulting system being able to mimic some desired behavior as specified by a system similar to S. A notion of on-line diagnosis is formulated which involves an external detector and a maximum time delay within which every error caused by a fault in a prescribed set must be detected. It is shown that if a system is on-line diagnosable for the unrestricted set of faults then the detector is at least as complex, in terms of state set size, as the specification. The use of inverse systems for the diagnosis of unrestricted faults is considered. A partial characterization of those inverses which can be used for unrestricted fault diagnosis is obtained.

  13. 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.

  14. 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.

  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. On-line solid phase extraction of Ni and Pb using carbon nanotubes and modified carbon nanotubes coupled to ETAAS.

    PubMed

    Savio, Marianela; Parodi, Belén; Martinez, Luis D; Smichowski, Patricia; Gil, Raúl A

    2011-07-15

    A study about the capabilities of three kinds of nanomaterials namely, carbon nanotubes (CNT), oxidized carbon nanotubes (ox-CNT) and l-alanine immobilized on carbon nanotubes (ala-CNT) to serve as sorbents for preconcentrating Ni and Pb using an on-line system coupled to electrothermal atomic absorption spectroscopy (ETAAS) technique, was accomplished. The solid phase extraction was performed in a conical minicolumn used as sorbent holder. After loading a fixed volume of the analytes, they were eluted with a discrete volume (50 μL) of nitric acid, placed directly into the platform of a L'Vov tube. After that, each analyte was determined individually. Ni and Pb retention was strongly influenced by pH but exhibiting different behaviors. The study demonstrated that the sorbent based on ox-CNTs was the one that exhibited the highest capacity and linearity for both analytes when compared with CNT or ala-CNT. The analytical performance was evaluated for the three sorbents to establish the best conditions regarding sensitivity, reproducibility and accuracy. The precision expressed as relative standard deviations (n=6) were 3.9 and 0.5% for Ni(2+) and Pb(2+), respectively The limit of detection (LOD), calculated as the concentration required to yield a net peak equal to three times the standard deviation of the background signal (3σ) was 30 and 10 ng L(-1) for Ni(2+) and Pb(2+) respectively. Alternatively, the limit of quantification (10σ) was calculated and resulted to be 0.79 and 0.07 μg L(-1) for Ni(2+) and Pb(2+) respectively. After optimization, the method that involved the use of ox-CNT associated to an on-line preconcentration was tested in samples of relevant environmental importance. Accuracy was evaluated analyzing a certified reference material namely, Municipal Sludge (QC MUNICIPAL SLUDGE A) and a reference sample of Lake Sediment (TRAP-LRM from IJS). PMID:21645695

  17. 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.

  18. On-line diagnosis of unrestricted faults

    NASA Technical Reports Server (NTRS)

    Meyer, J. F.; Sundstrom, R. J.

    1975-01-01

    Attention is given to the formal development of the notion of a discrete-time system and the associated concepts of fault, result of a fault, and error. The considered concept of on-line diagnosis is formalized and a diagnosis using inverse machines is discussed. The case of an inverse which is lossless is investigated. It is found that in such a case the class of unrestricted faults can be diagnosed with a delay equal to the delay of losslessness of the inverse system.

  19. Dairy Herd On-line Information System

    NASA Astrophysics Data System (ADS)

    Takahashi, Satoshi

    As the business circumstances have become worse, computational breeding management based on the scientific matters has been needed for dairy farming in our country. In this connection it was urgent to construct the system which provided data effectively used in the fields for dairy farmers. The Federation has executed to provide dairy farming technical data promptly through its own on-line network being composed of middle sized general-purpose computer (main memory : 5MB, and fixed disk : 1100MB) and 22 terminals.

  20. On-line and Mobil Learning Activities

    NASA Astrophysics Data System (ADS)

    Ackerman, S. A.; Whittaker, T. M.; Jasmin, T.; Mooney, M. E.

    2012-12-01

    Introductory college-level science courses for non-majors are critical gateways to imparting not only discipline-specific information, but also the basics of the scientific method and how science influences society. They are also indispensable for student success to degree. On-line, web-based homework (whether on computers or mobile devices) is a rapidly growing use of the Internet and is becoming a major component of instruction in science, replacing delayed feedback from a few major exams. Web delivery and grading of traditional textbook-type questions is equally effective as having students write them out for hand grading, as measured by student performance on conceptual and problem solving exams. During this presentation we will demonstrate some of the interactive on-line activities used to teach concepts and how scientists approach problem solving, and how these activities have impacted student learning. Evaluation of the activities, including formative and summative, will be discussed and provide evidence that these interactive activities significantly enhance understanding of introductory meteorological concepts in a college-level science course. More advanced interactive activities are also used in our courses for department majors, some of these will be discussed and demonstrated. Bring your mobile devices to play along! Here is an example on teaching contouring: http://profhorn.aos.wisc.edu/wxwise/contour/index.html

  1. The EINSTEIN On-Line Service (EOLS)

    NASA Astrophysics Data System (ADS)

    Harris, D. E.; Stern Grant, C. P.; Andernach, H.

    1994-08-01

    In January 1989, SAO established an on-line service to help astronomers prepare ROSAT proposals by providing access to the preliminary source list from the ``Einstein Observatory Catalog of IPC X-ray Sources''. In the intervening years, we have updated the source list, added to the documentation, included many more Einstein databases as well as a number of tables from other wavebands, provided access to images for downloading from all of the Einstein CDROMs, and installed new software for more sophisticated filtering and retrieval. Although we have improved the functionality and made significant additions to the databases, we still maintain a simple menu interface accessible from any type of terminal. EOLS provides all of our databases to the NASA Astrophysics Data System (ADS) and our documents which describe each table are thus written in the ADS format. In conjunction with the IAU working group on Archiving and Data Bases for Radio Astronomy, EOLS serves as an experimental platform for on-line access to the radio source lists collected by one of us (H.A.). The number of these entries exceeds half a million.

  2. Condenser on-line fouling monitor

    SciTech Connect

    Tsou, J.L.; Garey, J.F.; Wiebe, D.H.

    1994-12-31

    Biological and/or chemical fouling in utility condensers is a major cause of reduced efficiency and substantially affects availability and increases operational costs. Performance losses due to water side fouling are difficult to measure and, usually, quantitative assessment of the economic impact of condenser fouling is impossible. Plant operators typically examine steam backpressure and perform complex calculations for condenser cleanliness. These direct estimates are often imprecise due to inadequate instrumentation. In addition, these data provide information on overall condenser performance which may be influenced by a number of parameters which are independent of water side fouling. Indirect (side-stream) methods are also used to isolate/measure biological or chemical fouling in condensers. This approach is extremely useful to document site/seasonal fouling rates, and for the simultaneous evaluation of treatment options. In collaboration with the Electric Power Research Institute, instrumentation has been developed which meets requirements for the direct, on-line measurement of condenser fouling. This monitor may be installed in any location within the condenser, does not interfere with routine plant operations, including on-line mechanical and chemical treatment methods, and provides continuous, real-time readings of the heat transfer efficiency of the instrumented tube. Three prototype assemblies were installed at the New England Power Company, Brayton Point Generating Station in 1993. This paper discusses the design, construction, preliminary test results, and subsequent data collected in 1994 with a redesigned system.

  3. The design, fabrication and characterization of a silicon microheater for an integrated MEMS gas preconcentrator

    NASA Astrophysics Data System (ADS)

    Yeom, Junghoon; Field, Christopher R.; Bae, Byunghoon; Masel, Richard I.; Shannon, Mark A.

    2008-12-01

    We report the design and fabrication of a microheater unit as a key component of an integrated micro gas preconcentrator that has an ultra-small preconcentrator volume (<0.25 µL) and microvalves for fast injection speeds (<1 ms). Monolithic integration of the microvalves into the microheater of the preconcentrator gives rise to challenges in designing the microheater and implementing thermal isolation for low power and energy consumption. A preconcentrator chamber, 3.5 × 1.5 mm2 in planform area and 40 µm deep, was built in the device layer of a silicon-on-insulator wafer and filled with an array of microposts with a preconcentrator volume of 0.2-0.25 µL. Different generations of the microheaters and their mating dies were fabricated to show the effects of thermal isolation and thermal mass of the system on the performance of the heater. The microheater assembly with the least thermal mass and most thermal isolation can reach 300 °C in 100 ms with 12.3 W of power and is expected to consume less than 2 J during the operation of each preconcentration cycle.

  4. 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%.

  5. NASDA's Advanced On-Line System (ADOLIS)

    NASA Technical Reports Server (NTRS)

    Yamamoto, Yoshikatsu; Hara, Hideo; Yamada, Shigeo; Hirata, Nobuyuki; Komatsu, Shigenori; Nishihata, Seiji; Oniyama, Akio

    1993-01-01

    Spacecraft operations including ground system operations are generally realized by various large or small scale group work which is done by operators, engineers, managers, users and so on, and their positions are geographically distributed in many cases. In face-to-face work environments, it is easy for them to understand each other. However, in distributed work environments which need communication media, if only using audio, they become estranged from each other and lose interest in and continuity of work. It is an obstacle to smooth operation of spacecraft. NASDA has developed an experimental model of a new real-time operation control system called 'ADOLIS' (ADvanced On-Line System) adopted to such a distributed environment using a multi-media system dealing with character, figure, image, handwriting, video and audio information which is accommodated to operation systems of a wide range including spacecraft and ground systems. This paper describes the results of the development of the experimental model.

  6. On-line resources for Xenopus.

    PubMed

    Bowes, Jeff

    2012-01-01

    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

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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.

  12. Preconcentration method on modified silica fiber for chromium speciation.

    PubMed

    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

  13. 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

  14. 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

  15. 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

  16. On-Line Instruction: Are the Outcomes the Same?

    ERIC Educational Resources Information Center

    Warren, Louis L.; Holloman, Harold L., Jr.

    2005-01-01

    Institutions of higher education are offering more and more on-line courses to students. Do students receive the same quality of instruction with an on-line class as an on-campus class? Specifically, is there a difference in students' outcomes between a face-to-face class and on-line class? This study addresses that question by collecting and…

  17. 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…

  18. An Evaluation of On-Line Information Retrieval System Techniques.

    ERIC Educational Resources Information Center

    Wolfe, Theodore

    This report presents a review and evaluation of three remote access on-line information retrieval systems and some ideas on what the capabilities of an ideal on-line information retrieval system should be. The three systems reviewed are the DDC Remote On-Line Retrieval System, the National Aeronautics and Space Administration RECON System, and the…

  19. 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.

  20. 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...

  1. On-line sample preconcentration by sweeping and poly(ethylene oxide)-mediated stacking for simultaneous analysis of nine pairs of amino acid enantiomers in capillary electrophoresis.

    PubMed

    Lin, En-Ping; Lin, Kai-Cheng; Chang, Chia-Wei; Hsieh, Ming-Mu

    2013-09-30

    This study proposes a sensitive method for the simultaneous separation and concentration of 9 pairs of amino acid enantiomers by combining poly(ethylene oxide) (PEO)-based stacking, β-cyclodextrin (β-CD)-mediated micellar electrokinetic chromatography (MEKC), and 9-fluoroenylmethyl chloroformate (FMOC) derivatization. The 9 pairs of FMOC-derivatized amino acid enantiomers were baseline separated using a discontinuous system, and the buffer vials contained a solution of 150 mM Tris-borate (TB), 12.5% (v/v) isopropanol (IPA), 0.5% (w/v) PEO, 35 mM sodium taurodeoxycholate (STDC), and 35 mM β-CD, and the capillary was filled with a solution of 1.5 M TB, 12.5% (v/v) IPA, 35 mM STDC, and 35 mM β-CD. Based on the difference in viscosity between the sample zone and PEO solution and because of the STDC sweeping, the discontinuous system effectively stacked 670 nL of the 9 pairs of FMOC-derivatized amino acid enantiomers without losing chiral resolution. Consequently, the limits of detection for the 9 pairs of FMOC-derivatized amino acid enantiomers were reduced to 40-60 nM. This method was successfully used to determine d-Tryptophan (Trp), l-Trp, d-Phenylalanine (Phe), l-Phe, d-Glutamic acid (Glu), and l-Glu in various types of beers. PMID:23953474

  2. 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...

  3. On-line evaluation of multiloop digital controller performance

    NASA Technical Reports Server (NTRS)

    Wieseman, Carol D.

    1993-01-01

    The purpose of this presentation is to inform the Guidance and Control community of capabilities which were developed by the Aeroservoelasticity Branch to evaluate the performance of multivariable control laws, on-line, during wind-tunnel testing. The capabilities are generic enough to be useful for all kinds of on-line analyses involving multivariable control in experimental testing. Consequently, it was decided to present this material at this workshop even though it has been presented elsewhere. Topics covered include: essential on-line analysis requirements; on-line analysis capabilities; on-line analysis software; frequency domain procedures; controller performance evaluation frequency-domain flutter suppression; and plant determination.

  4. Students On-Line Atmospheric Research

    NASA Astrophysics Data System (ADS)

    Woods, D. C.; Moore, S. W.; Walters, S. C.

    2002-12-01

    Students On-Line Atmospheric Research (SOLAR) is one of NASA's educational outreach programs. SOLAR's primary role is to support educational outreach activities for NASA's Stratospheric Aerosol and Gas Experiment III (SAGE III). SAGE III is the latest version of a series of solar occultation experiments, which include SAGE I and SAGE II. The SAGE III instrument was launched on a Russian METEOR 3M spacecraft in December 2001, and is now monitoring the global distribution of aerosols, ozone, clouds, and other important trace gases in the upper atmosphere. The SAGE measurements are critical to improving the understanding of global climate forcing as well as atmospheric chemical processes in the upper atmosphere. The SAGE experiment addresses interesting science problems related to the Earth's atmosphere. Many exciting science and technology topics from SAGE can be developed and incorporated into K-12 curriculum materials to enhance student interest in science. In addition, technologies employed by the SAGE measurement technique give rise to ideas for science projects that involve student participation. The SOLAR outreach program helps to bring these topics and ideas to the classroom by focusing on helping teachers become familiar with current research in the atmospheric sciences, and helping them integrate SOLAR developed educational materials into their curriculum. SOLAR gives special presentations at national and regional science teacher conferences and conducts an annual summer teacher workshop at the NASA Langley Research Center. Members of the SOLAR team also visit schools give classroom presentations and presentations to special student groups. This poster highlights some of the key features of the SOLAR program and presents descriptions of student projects, teacher workshops, and SOLAR resources.

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

    PubMed

    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. PMID:26471041

  6. 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.

  7. 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.

  8. 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

  9. Methane preconcentration in a microtrap using multiwalled carbon nanotubes as sorbents.

    PubMed

    Saridara, Chutarat; Ragunath, Smruti; Pu, Yong; Mitra, Somenath

    2010-09-10

    The GC monitoring of green house gases is a challenging task because the concentration of organic species such as methane are relatively low (ppm to ppb) and their analysis requires some level of preconcentration. Since methane is highly volatile, it is not easily retained on conventional sorbents. In this paper we present multiwalled carbon nanotubes (MWNTs) as an effective sorbent for a microtrap designed for methane preconcentration. Its performance was compared to other commercially available carbon based sorbents, and it was found to be the most effective sorbent in terms of breakthrough volume and enthalpy of adsorption. PMID:20850589

  10. 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.

  11. Paper-Based Flow Fractionation System Applicable to Preconcentration and Field-Flow Separation.

    PubMed

    Hong, Seokbin; Kwak, Rhokyun; Kim, Wonjung

    2016-02-01

    We present a novel paper-based flow fractionation system for preconcentration and field-flow separation. In this passive fluidic device, a straight channel is divided into multiple daughter channels, each of which is connected with an expanded region. The hydrodynamic resistance of the straight channel is predominant compared with those of expanded regions, so we can create steady flows through the straight and daughter channels. While the expanded regions absorb a great amount of water via capillarity, the steady flow continues for 10 min without external pumping devices. By controlling the relative hydrodynamic resistances of the daughter channels, we successfully divide the flow with flow rate ratios of up to 30. Combining this bifurcation system with ion concentration polarization (ICP), we develop a continuous-flow preconcentrator on a paper platform, which can preconcentrate a fluorescent dye up to 33-fold. In addition, we construct a field-flow separation system to divide two different dyes depending on their electric polarities. Our flow fractionation systems on a paper-based platform would make a breakthrough for point-of-care diagnostics with specific functions including preconcentration and separation. PMID:26713779

  12. 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. PMID:22780835

  13. 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 ...

  14. 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. PMID:25372369

  15. Paper-based flow fractionation system for preconcentration and field-flow fractionation.

    NASA Astrophysics Data System (ADS)

    Hong, Seokbin; Kwak, Rhokyun; Kim, Wonjung

    2015-11-01

    We present a novel paper-based flow fractionation system for preconcentration and field-flow fractionation. The paper fluidic system consisting of a straight channel connected with expansion regions can generate a fluid flow with a constant flow rate for 10 min without any external pumping devices. The flow bifurcates with a fraction ratio of up to 30 depending on the control parameters of the channel geometry. Utilizing this simple paper-based bifurcation system, we developed a continuous-flow preconcentrator and a field-flow fractionator on a paper platform. Our experimental results show that the continuous-flow preconcentrator can produce a 33-fold enrichment of the ion concentration and that the flow fractionation system successfully separates the charged dyes. Our study suggests simple, cheap ways to construct preconcentration and field-flow fractionation systems for paper-based microfluidic diagnostic devices. This work was supported by the National Research Foundation of Korea(NRF) grant funded by the Korea government(MSIP) (NRF-2015R1A2A2A04006181).

  16. On-Line Distance Learning: A Model for Developing Countries.

    ERIC Educational Resources Information Center

    Khan, Abdul W.

    2000-01-01

    Discusses issues related to open and distance-learning (ODL) in developing countries, using the virtual campus initiative of the Indira Gandhi National Open University (India) as an example and model of on-line program delivery and on-line, for-profit telelearning centers. Suggests strategies to enable open and distance-learning institutions to…

  17. Issues Affecting Teaching On-Line: An Annotated Bibliography.

    ERIC Educational Resources Information Center

    Thompson, Kelvin

    This annotated bibliography identifies issues affecting the on-line teaching environment by assembling a variety of quantitative and qualitative studies. Studies in the bibliography are divided into two major categories: (1) topical studies, which contain papers that focus primarily on one issue affecting teaching on-line (student…

  18. Chat: The Missing Link in On-Line Instruction.

    ERIC Educational Resources Information Center

    Roberson, Thelma J.; Klotz, Jack

    As more courses in higher education move to an on-line format, a major concern that has arisen is the lack of personal interaction between the professor and student. The literature provides evidence that often on-line courses are configured and delivered in a style more often associated with independent study or correspondence work, i.e., students…

  19. 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…

  20. 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...

  1. On-Line Administrative Information Systems: A Case Study.

    ERIC Educational Resources Information Center

    Sire, Paul W.

    A case study approach is used to document the on-line information system developed by the Office of Management Information and Computing at the University of Vermont. Stanford University's Project INFO On-Line Administration Information System, OASIS, was chosen as a model. The administrative system is one of two on campus, the other designed for…

  2. 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…

  3. 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…

  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. 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…

  6. 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…

  7. Dynamic layer-by-layer self-assembly of multi-walled carbon nanotubes on quartz wool for on-line separation of lysozyme in egg white.

    PubMed

    Du, Zhuo; Zhang, Suling; Zhou, Chanyuan; Liu, Miao; Li, Gongke

    2012-05-30

    The multi-walled carbon nanotubes (MWNTs) coated quartz wool (MWNTs/QW) prepared by dynamic layer-by-layer self-assembly was used as solid-phase extraction (SPE) absorbent for on-line separation and preconcentration of lysozyme in egg white. The coating procedures were performed continuously in a flow system operated by a set of sequential injection devices. The quartz wool was placed in a microcolumn forming a loose packing to guarantee the minimized flow impedance and the intimate contact between proteins and absorbent surface. Various parameters affecting SPE efficiency including the volume, pH, ionic strength and flow rate of sample and eluent were systematically studied. The feasibility of the proposed method was validated by successfully applied to the separation of lysozyme in egg white. PMID:22608421

  8. Evaluation of a Reactor On-Line Uncertainty Monitoring System

    SciTech Connect

    Edwards, Robert M.; He, Weidong

    2001-06-17

    Robust control designs were developed to better match experimental conditions available in the TRIGA reactor. A first-order weighting function is specified for each operating range in the robust design to limit the maximum tracking error. Inclusion of the performance-weighting function as the on-line filter is discussed as a possible on-line performance-monitoring method. The scheme to evaluate an on-line uncertainty monitoring system for a robust reactor controller is shown. TRIGA reactor experiments were conducted to evaluate on-line performance-monitoring techniques. It is concluded that the observed robust-control performance-monitoring characteristics can be incorporated in an on-line decision-making process to choose appropriate robust control selection and enforcement.

  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. 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

    Zereen, Fahmida; Yilmaz, Vedat; Arslan, Zikri

    2014-01-01

    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

  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. On-Line Allocation Of Robot Resources To Task Plans

    NASA Astrophysics Data System (ADS)

    Lyons, Damian M.

    1989-02-01

    In this paper, I present an approach to representing plans that make on-line decisions about resource allocation. An on-line decision is the evaluation of a conditional expression involving sensory information as the plan is being executed. I use a plan representation called 7ZS10'1 1,12that has been especially designed for the domain of robot programming, and in particular, for the problem of on-line decisions. The resource allocation example is based on the robot assembly cell architecture outlined by Venkataraman and Lyons16. I begin by setting forth a definition of on-line decision making and some arguments as to why this form of decision making is important and useful. To set the context for the resource allocation example, I take some care in categorizing the types of on-line decision making and the approaches adopted by other workers so far. In particular, I justify a plan-based approach to the study of on-line decision making. From that, the focus shifts to one type of decision making: on-line allocation of robot resources to task plans. Robot resources are the physical manipulators (grippers, wrists, arms, feeders, etc) that are available to carry out the task. I formulate the assembly cell architecture of Venkataraman and Lyons16 as an R.S plan schema, and show how the on-line allocation specified in that architecture can be implemented. Finally, I show how considering the on-line allocation of logical resources, that is a physical resource plus some model information, can be used as a non-traditional approach to some problems in robot task planning.

  13. Practical experience with on-line ion chromatography

    SciTech Connect

    Lynch, G.J.

    1991-12-31

    Bettis is heavily involved in on-line ion chromatography and has gained much experience with the systems. This paper serves to pass that experience along to any users, current or prospective, that are interested in the systems. On-line IC is extremely dynamic and the developments over the past few years have helped to produce systems that can provide technical and productivity improvements. The potential uses of the systems are only beginning to be tapped. It is the information provided herein maybe useful to any interested in on-line ion chromatography.

  14. Flow injection on-line solid phase extraction coupled with inductively coupled plasma mass spectrometry for determination of (ultra)trace rare earth elements in environmental materials using maleic acid grafted polytetrafluoroethylene fibers as sorbent.

    PubMed

    Wang, Zhao-Hui; Yan, Xiu-Ping; Wang, Zhi-Peng; Zhang, Zheng-Pu; Liu, Li-Wen

    2006-09-01

    A new sorbent, maleic acid grafted polytetrafluoroethylene fiber (MA-PTFE), was prepared and evaluated for on-line solid-phase extraction coupled with inductively coupled plasma mass spectrometry (ICP-MS) for fast, selective, and sensitive determination of (ultra)trace rare earth elements (REEs) in environmental samples. The REEs in aqueous samples at pH = 3.0 were selectively extracted onto a microcolumn packed with the MA-PTFE fiber, and the adsorbed REEs were subsequently eluted on-line with 0.9 mol l(-1) HNO3 for ICP-MS determination. The new sorbent extraction system allows effective preconcentration and separation of the REEs from the major matrix constituents of alkali and alkali earth elements, particularly their separation from barium that produces considerable isobaric interferences of 134Ba16O1H+, 135Ba16O+, 136Ba16O1H+, and 137Ba16O+ on 151Eu+ and 153Eu+. With the use of a sample loading flow rate of 7.4 ml min(-1) for 120 s preconcentration, enhancement factors of 69-97 and detection limits (3s) of 1-20 pg l(-1) were achieved at a sample throughput of 22 samples h(-1). The precision (RSD) for 16 replicate determinations of 50 ng l(-1) of REEs was 0.5-1.1%. The developed method was successfully applied to the determination of (ultra)trace REEs in sediment, soil, and seawater samples. PMID:16814561

  15. Determination of quinolones and fluoroquinolones in hospital sewage water by off-line and on-line solid-phase extraction procedures coupled to HPLC-UV.

    PubMed

    Turiel, Esther; Bordin, Guy; Rodríguez, Adela Rosa

    2005-02-01

    In this work, the development of two solid-phase extraction procedures (off-line and on-line formats) for the identification and quantification of several (fluoro)quinolones in hospital sewage water by HPLC-UV is described. Both procedures are based on the use of C18 and anion exchange (SAX) sorbents for the preconcentration and clean-up steps, respectively, and all variables influencing both steps were optimised. In the off-line format, after its pH was adjusted to 2.5, sample was preconcentrated on a C18 cartridge and eluted with 4 mL of methanol/ammonia (94/6). The methanolic extract must be diluted up to 10 mL with water to allow quantitative retention of the analytes on the SAX cartridge. In the on-line format, the addition of 2.5% of NH4Cl to the sewage water sample (pH = 2.5) was necessary to increase the breakthrough volumes of the analytes in the C18 precolumn. Quantitative transfer of the (fluoro)quinolones from the C18 precolumn to the SAX precolumn was accomplished by pumping 2 mL of a mixture methanol/water (40/60, pH = 9.2) at 2 mL min(-1). Elution of the analytes from the SAX precolumn by means of the chromatographic mobile phase required the inclusion of an additional isocratic step at the beginning of the gradient program. Both off-line and on-line solid phase extraction procedures coupled to HPLC-UV were applied to the analysis of a sewage water sample collected in the sewer system at the output of the St Dimphna Hospital (Geel, Belgium). The fluoroquinolone ciprofloxacin was found in this sample and quantified at 5.8 +/- 0.4 microg L(-1) (off-line method) and 5.6 +/- 0.5 microg L(-1) (on-line method). The analysis of spiked samples containing the seven (fluoro)quinolones studied provided quantitative recoveries in all cases with low RSD values (from 6 to 12%), and all the analytes could be identified by means of their UV spectra with match factors varying from 950 to 985 depending on the (fluoro)quinolone. PMID:15776928

  16. 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)

  17. Recent Advances in On-Line Methods Based on Extraction for Speciation Analysis of Chromium in Environmental Matrices.

    PubMed

    Trzonkowska, Laura; Leśniewska, Barbara; Godlewska-Żyłkiewicz, Beata

    2016-07-01

    The biological activity of Cr(III) and Cr(VI) species, their chemical behavior, and toxic effects are dissimilar. The speciation analysis of Cr(III) and Cr(VI) in environmental matrices is then of great importance and much research has been devoted to this area. This review presents recent developments in on-line speciation analysis of chromium in such samples. Flow systems have proved to be excellent tools for automation of sample pretreatment, separation/preconcentration of chromium species, and their detection by various instrumental techniques. Analytical strategies used in chromium speciation analysis discussed in this review are divided into categories based on selective extraction/separation of chromium species on solid sorbents and liquid-liquid extraction of chromium species. The most popular strategy is that based on solid-phase extraction. Therefore, this review shows the potential of novel materials designed and used for selective binding of chromium species. The progress in miniaturization of measurement systems is also presented. PMID:26186521

  18. 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

  19. 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

  20. Nafion Film Based Micro-nanofluidic Device for Concurrent DNA Preconcentration and Separation in Free Solution

    PubMed Central

    Song, Hongjun; Wang, Yi; Garson, Charles; Pant, Kapil

    2014-01-01

    This paper presents a Nafion film based micro-nanofluidic device for concurrent DNA preconcentration and separation. The principle of the device is based on the combination of (a) ion concentration polarization phenomenon at the junction of the microchannel and the nanochannels in the Nafion film to form opposing electrophoretic and electroosmotic forces acting on the DNAs, and (b) end-labeled free solution electrophoresis to harness the charge-to-mass ratio for molecular differentiation. The experiments successfully demonstrated concurrent preconcentration and separation of DNA mixture in free solution within 240s, yielding concentration ratios up to 1,150X and separation resolution of 1.85. The effect of applied electric field on the concentration and separation performance was also investigated. The device can be used as a key sample preparation element in conjunction with micro- or nano-fluidic sensors for microTAS functionality. PMID:25346656

  1. From carbon nanostructures to high-performance sorbents for chromatographic separation and preconcentration

    NASA Astrophysics Data System (ADS)

    Postnov, V. N.; Rodinkov, O. V.; Moskvin, L. N.; Novikov, A. G.; Bugaichenko, A. S.; Krokhina, O. A.

    2016-02-01

    Information on carbon nanostructures (fullerenes, nanotubes, graphene, nanodiamond and nanodispersed active carbon) used to develop high-performance sorbents of organics and heavy metal ions from aqueous solutions is collected and analyzed. The advantages in the synthesis of hybrid carbon nanostructures and the possibilities of surface modification of these systems in order to carry out fast sorption pre-concentration are considered. Prospects for application of these materials in sorption technologies and analytical chemistry are discussed. The bibliography includes 364 references.

  2. Determination of actinides in environmental samples using an automated batch preconcentration/matrix elimination system

    SciTech Connect

    Smith, F.G.; Crain, J.S.

    1995-12-31

    The determination of thorium, uranium, and uranium progeny (e.g. {sup 226}Ra) in environmental samples is of considerable interest in terms of human health. Traditional radiochemical determinations of long-lived radioisotopes often require rigorous chemical separations and long duration measurements by techniques such as {alpha}-spectrometry. Inductively coupled plasma mass spectrometry (ICP-MS) offers sub-ppt (1 ng/L) detection limits for the actinides with minimal sample preparation and high sample throughput. However, sample preconcentration and/or matrix elimination is required to achieve required detection limits below 1ppq (1 pg/L). This paper describes a batch preconcentration/matrix elimination system for off-line sample preparation. An aliquot of an actinide selective polymer beads is added to a sample and pumped through a filter. Unbound sample matrix components are washed to waste then the beads with bound actinides are released in a small volume. The preconcentrate is then introduced to the ICP-MS by pneumatic or ultrasonic nebulization. Data for a variety of natural water matrices (well, spring, lake, river, and tapwater) will be presented.

  3. Preconcentration and determination of tellurium in garlic samples by hydride generation atomic absorption spectrometry.

    PubMed

    Kaplan, Marcos M; Cerutti, Soledad; Salonia, José A; Gásquez, José A; Martinez, Luis D

    2005-01-01

    A procedure for the determination of traces of total tellurium (Te) in garlic (Allium sativa) is described that combines hydride generation atomic absorption spectrometry with preconcentration of the analyte by coprecipitation. The samples, each spiked with lanthanum nitrate (20 mg/L), are introduced into an Amberlite XAD-4 resin and mixed with ammonium buffer (pH 9.1). Te is preconcentrated by coprecipitation with the generated lanthanum hydroxide precipitate. The precipitate is quantitatively collected in the resin, eluted with hydrochloric acid, and then transferred into the atomizer device. Considering a sample consumption of 25 mL, an enrichment factor of 10 was obtained. The detection limit (3sigma) was 0.03 microg/L, and the precision (relative standard deviation) was 3.5% (n = 10) at the 10 microg/L level. The calibration graph using the preconcentration system for Te was linear with a correlation coefficient of 0.9993. Satisfactory results were obtained for the analysis of Te in garlic samples. PMID:16152948

  4. Flow-Injection Preconcentration of Chloramphenicol Using Molecularly Imprinted Polymer for HPLC Determination in Environmental Samples

    PubMed Central

    Kowalski, Damian; Poboży, Ewa; Trojanowicz, Marek

    2011-01-01

    The residue of antibiotic chloramphenicol (CAP) is important issue for food quality control and also for the environmental monitoring. It is banned for use in food-producing animals and has very limited use in human medicine, because of its severe impact on human health. Determination of trace level of CAP in environmental samples requires a very sensitive analytical method and efficient preconcentration procedure. CAP can be efficiently preconcentrated in flow-injection system using flow-through reactor packed with molecularly imprinted polymer (MIP), but determination of CAP in eluate from MIP requires the application of chromatographic separation, which was made in reversed-phase HPLC system with UV detection. In optimized conditions the limit of detection for 100 mL sample in HPLC with offline preconcentration on MIP was evaluated as 0.66 mg/L. In hyphenated FIA-HPLC system with zone sampling the LOD for developed method was evaluated as 15 ng/L, which indicates the possibility of using it for analysis of environmental samples. PMID:21584273

  5. Preconcentration of some metal ions with lanthanum-8-hydroxyquinoline co-precipitation system.

    PubMed

    Feist, Barbara; Mikula, Barbara

    2014-03-15

    A method of separation and preconcentration of cadmium, copper, nickel, lead and zinc at trace level using 8-hydroxyquinoline as a chelating agent and lanthanum(III) as a carrier element is proposed. The heavy metals were determined after preconcentration by inductively coupled plasma optical emission spectrometry (ICP-OES). The results were compared with those obtained using flame atomic absorption spectrometry (F-AAS). The influence of several parameters such as pH, amount of lanthanum(III) as a carrier element, amount of 8-hydroxyquinoline, duration of co-precipitation was examined. Moreover, effects of inorganic matrix on recovery of the determined elements were studied. The detection limits (DL) for ICP-OES were 0.31, 2.9, 1.4, 3.2 and 1.2 μg L(-1) for Cd, Cu, Ni, Pb and Zn, respectively, whereas for F-AAS DL were 0.63, 1.1, 3.2, 2.7 and 0.74 μg L(-1). The recovery of the method for the determined elements was better than 94% with relative standard deviation between 0.63% and 2.9%. The preconcentration factor was 60. The proposed method was successfully applied for determination of Cd, Cu, Ni, Pb, and Zn in plant materials. Accuracy of the proposed method was verified using certified reference material (NCS ZC85006 Tomato). PMID:24206710

  6. 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

  7. Combination of in situ preconcentration and on-site analysis for phosphate monitoring in fresh waters.

    PubMed

    Li, Weijia; Lee, Lai Yoke; Yung, Lin Yue Lanry; He, Yiliang; Ong, Choon Nam

    2014-08-01

    Excess nutrients of phosphorus and nitrogen would lead to adverse impacts on a water body. It is important that their concentrations in a dynamic water ecosystem are measured accurately and constantly for an early warning before occurrences of algal blooms and for environmental management. Nevertheless, on-site measurements by existing technologies are often limited by the inherent sensitivities. In this study, a portable system for dissolved phosphate monitoring in freshwater based on the diffusive gradients in thin films (DGT) technique was developed. A polydiallydimethylammonium chloride (PDA) aqueous solution and a dialysis membrane were used as a binding phase and a diffusive layer in this preconcentration device, respectively. The binding properties of the PDA solution were evaluated in solutions of different pH (3 to 9) and varying concentrations of anions (2.0-20 mM). The amount of phosphates preconcentrated in the devices was measured by ultraviolet-visible (UV) spectroscopy to obtain the concentrations in waters without elution steps. The devices were validated in synthetic river water with good agreement with the theoretical prediction and in natural river water. A system combining this preconcentration device and a compact detection chamber equipped with a pair of light emitting diodes (LED) was studied in lab synthetic solutions for on-site monitoring of phosphate concentrations and their fluctuations. PMID:25011428

  8. Solid-Nanoemulsion Preconcentrate for Oral Delivery of Paclitaxel: Formulation Design, Biodistribution, and γ Scintigraphy Imaging

    PubMed Central

    Ahmad, Javed; Mir, Showkat R.; Kohli, Kanchan; Chuttani, Krishna; Mishra, Anil K.; Panda, A. K.

    2014-01-01

    Aim of present study was to develop a solid nanoemulsion preconcentrate of paclitaxel (PAC) using oil [propylene glycol monocaprylate/glycerol monooleate, 4 : 1 w/w], surfactant [polyoxyethylene 20 sorbitan monooleate/polyoxyl 15 hydroxystearate, 1 : 1 w/w], and cosurfactant [diethylene glycol monoethyl ether/polyethylene glycol 300, 1 : 1 w/w] to form stable nanocarrier. The prepared formulation was characterized for droplet size, polydispersity index, and zeta potential. Transmission electron microscopy (TEM), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR) were used to assess surface morphology and drug encapsulation and its integrity. Cumulative drug release of prepared formulation through dialysis bag and permeability coefficient through everted gut sac were found to be remarkably higher than the pure drug suspension and commercial intravenous product (Intaxel), respectively. Solid nanoemulsion preconcentrate of PAC exhibited strong inhibitory effect on proliferation of MCF-7 cells in MTT assay. In vivo systemic exposure of prepared formulation through oral administration was comparable to that of Intaxel in γ scintigraphy imaging. Our findings suggest that the prepared solid nanoemulsion preconcentrate can be used as an effective oral solid dosage form to improve dissolution and bioavailability of PAC. PMID:25114933

  9. Concurrent DNA Preconcentration and Separation in Bipolar Electrode-Based Microfluidic Device

    PubMed Central

    Song, Hongjun; Wang, Yi; Garson, Charles; Pant, Kapil

    2015-01-01

    This paper presents a bipolar electrode (BPE) device in a microfluidic dual-channel design for concurrent preconcentration and separation of composite DNA containing samples. The novelty of the present effort relies on the combination of BPE-induced ion concentration polarization (ICP) and end-labeled free-solution electrophoresis (ELFSE). The ion concentration polarization effect arising from the faradaic reaction on the BPE is utilized to exert opposing electrophoretic and electroosmotic forces on the DNA samples. Meanwhile, end-labeled free-solution electrophoresis alters the mass-charge ratio to enable simultaneous DNA separation in free solution. The microfluidic device was fabricated using standard and soft lithography techniques to form gold-on-glass electrode capped with a PDMS microfluidic channel. Experimental testing with various DNA samples was carried out over a range of applied electric field. Concentration ratios up to 285× within 5 minutes for a 102-mer DNA, and concurrent preconcentration and free-solution separation of binary mixture of free and bound 102-mer DNA within 6 minutes was demonstrated. The effect of applied electric field was also interrogated with respect to pertinent performance metrics of preconcentration and separation. PMID:26005497

  10. 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.

  11. 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.

  12. Fundamentals of on-line gauging for machine vision

    NASA Astrophysics Data System (ADS)

    Novini, Amir R.

    1991-09-01

    This paper addresses the major issues in the application of machine-vision technology as an in- process, noncontact gauging tool on the factory floor. This includes the following: (1) How can machine vision be used for an on-line gauging application? (2) What is means by the terms resolution, accuracy, repeatability, and tolerance? How do they relate to each other? (3) What are the imaging concerns, part-edge qualities, back lighting versus front lighting, TV camera usage, optical consideration, and telecentric lens (constant magnification lens)? (4) What is meant by subpixel resolution and accuracy? How can it be achieved? (5) What are the practical limits for on-line industrial machine vision gauging application? The above questions are put into perspective by examining existing applications of on-line machine-vision gauging systems.

  13. 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. PMID:11246921

  14. 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

  15. On-line pre-reduction of pentavalent arsenicals by thioglycolic acid for speciation analysis by selective hydride generation cryotrapping atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Musil, Stanislav; Matoušek, Tomáš

    2008-06-01

    An improvement of current method of selective hydride generation based on pre-reduction for differentiation of tri- and pentavalent arsenicals is described, applied for the oxidation state specific speciation analysis of inorganic, mono-, di- and trimethylated arsenicals with minimum sample pretreatment using atomic absorption spectrometry with the multiatomizer. The preconcentration and separation of arsine, methylarsine, dimethylarsine and trimethylarsine are then carried out by means of cryotrapping. The presented study shows that 2% (m/v) L-cysteine hydrochloride monohydrate ( L-cys) currently used for off-line pre-reduction of pentavalent arsenicals can be substituted with 1% (m/v) thioglycolic acid (TGA). Much faster pre-reduction of pentavalent arsenicals at 25 °C with equal sensitivities as in the case of L-cys has been achieved with TGA. A setup for on-line pre-reduction by TGA has been optimized, with the application of segmented flow analysis for suppression of axial dispersion in the pre-reduction coil. Standard calibrations measured with or without on-line pre-reduction indicate uniform and equal sensitivities for all As forms. The possibility of standardization by water standards of single species (e.g. iAs(III)) for quantification of all other As forms in urine is demonstrated in the recovery study. Limits of detection were 100 ng l - 1 for iAs(III), 135 ng l - 1 for iAs(V) and 30 to 50 ng l - 1 for methylated arsenicals.

  16. 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

  17. Characterizing the Performance of a Proton-Transfer-Reaction Mass Spectrometer with a Rapid Cycling Tenax Preconcentrator

    SciTech Connect

    Garland, S.P.; Alexander, M.L.

    2006-01-01

    Volatile organic compounds (VOCs) are species of interest for atmospheric modeling, worker chemical exposure and medical studies. Sometimes the required detection limits for these compounds is below the capability of existing real-time instrumentation. Preconcentrators have been implemented as an inexpensive way to amplify chemical signals and improve detection limits. Proton-transfer-reaction mass spectrometry (PTR-MS) has been used as a tool for studying low concentrations of VOCs, but it lacks the capability to differentiate chemical signal contributions from isobaric compounds. In this work, behavior of a newly designed Tenax TA preconcentrator when coupled with a PTRMS is characterized. This novel preconcentrator design allows rapid temperature cycling, maintaining near real-time response. The preconcentrator was exposed to a sample gas of toluene in varying concentrations and loading times between and then thermally desorbed for analysis by PTR-MS. The effects of preconcentrating multiple analytes simultaneously were also investigated as well as the chromatographic effects of the preconcentrator. A linear behavior was observed when the integrated ion count rates (ICPS) from thermal desorption peaks were regressed against both varying loading times at a constant toluene concentration and varying concentrations with constant loading times. From these trends, it is possible to determine the concentration of a VOC by knowing its ICPS from thermal desorption peaks from a known preconcentration time. Peak height ion count rates representing ultimate detectability were amplified by factors up to 257 times the original signal, extending the range of the PTR-MS from 50pptv to nearly 250 parts per quadrillion. This corresponds to an ultimate sensitivity of 200 parts per quadrillion with 20 minute time resolution. Quantitative preconcentrator behavior was demonstrated using ICPS from these ion peaks and were amplified as much as 148 times their original signal. Results

  18. Assessment of an On-Line Educational Administration Course

    ERIC Educational Resources Information Center

    Kim, Lori

    2004-01-01

    An on-line education administration course was evaluated using Seven Lessons Learned by Graham, Cagiltay, Lim, Craner, and Duffy (2001 ) as the framework. The framework was found to be useful in revealing areas of strengths and weaknesses in offering virtual education administration courses. The evaluation provided information that clear…

  19. Using On-line Corpus To Facilitate Language Learning.

    ERIC Educational Resources Information Center

    Sun, Yu-Chih

    The potential for on-line corpus in language teaching and learning has been the focus of attention on the part of teachers and researchers for some time now. The purpose of this study is to report on an Internet-based concordance approach to language learning and to investigate both qualitatively and quantitatively Taiwanese…

  20. 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…

  1. On-Line Schemes For Computing Rotation Angles For SVDS

    NASA Astrophysics Data System (ADS)

    Ercegovac, Milos D.; Lang, Tomas

    1988-01-01

    Two floating-point radix-2 schemes using on-line arithmetic for implementing the direct two-angle method for SVDs are presented. The first scheme is an on-line variant of the cosine/sine approach and is the fastest of the schemes considered: it performs the 2x2 SVD step in about 2n clock cycles. However, it requires a relatively large number of modules; this number is reduced when some modules are reused, resulting in a time of 3n clock cycles. The number of modules of this on-line version is still larger than that of the conventional one, but this is compensated by the smaller number of bit-slices per module and by the digit-serial communication among modules. The corresponding speed-up ratios are of 5 and 3 with respect to a conventional arithmetic implementation. The second scheme uses an on-line CORDIC approach and performs the 2x2 SVD in about 7n clock cycles and is advantageous because it is more time-area efficient. It results in a speed-up of about 2.5 with respect to the conventional CORDIC implementation.

  2. 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…

  3. Towards a Rhetoric of On-line Tutoring.

    ERIC Educational Resources Information Center

    Coogan, David

    Electronic mail-based tutoring of undergraduate writing students upsets the temporal basis of the face-to-face paradigm for writing tutorials. Taking place in real time in a specified place, the face-to-face tutorial session has a beginning, middle and end. Further, the session must have a tangible point. By contrast, in on-line tutoring, time is…

  4. An Experimental On-Line Information Retrieval System.

    ERIC Educational Resources Information Center

    Cautin, Harvey; And Others

    This paper reports an experiment in on-line retrieval using man-machine dialogue on a remote console. Message editing procedures and the use of two command languages are described. The system employs a PDP-8 computer for generating, proofreading, and editing messages, and an IBM 7040 computer for information retrieval processing. The symbolic…

  5. The On-Line Processing of Written Irony

    ERIC Educational Resources Information Center

    Filik, Ruth; Moxey, Linda M.

    2010-01-01

    We report an eye-tracking study in which we investigate the on-line processing of written irony. Specifically, participants' eye movements were recorded while they read sentences which were either intended ironically, or non-ironically, and subsequent text which contained pronominal reference to the ironic (or non-ironic) phrase. Results showed…

  6. 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 ...

  7. 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…

  8. 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…

  9. BCN: On-Line Information Retrieval for the Masses?

    ERIC Educational Resources Information Center

    Hess, Edward J.

    On-line information retrieval systems will spread beyond its narrow scope with the widespread development of interactive communication capability in connection with cable television. There is a possibility of far better attention to the information needs of the non-specialist with a coordinated information source. The major problems of such a…

  10. 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…

  11. 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.

  12. Growing Academic Vocabulary with a Collaborative On-Line Database.

    ERIC Educational Resources Information Center

    Cobb, Tom; Horst, Marlise

    This paper examines how collaborative on-line databases can be used to meet the need for individualized instruction for academic vocabulary learners intending to do university work in English. It is argued that effective teaching and course design for preparing non-native English speaking students for study at English language universities must be…

  13. 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

  14. 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…

  15. 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…

  16. On-Line Text Processing: Introduction and Overview.

    ERIC Educational Resources Information Center

    Walker, D.E.

    The objective of the current work program is to develop an on-line computer capability that would assist an information analyst in processing textual materials. The initial result of the work program is the design of a system for text processing and a computer implementation of a preliminary model of the system that strongly supports the validity…

  17. 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…

  18. On-line fuzzy logic control of tube bending

    NASA Astrophysics Data System (ADS)

    Lieh, Junghsen; Li, Wei Jie

    2005-11-01

    This paper describes the simulation and on-line fuzzy logic control of tube bending. By combining elasticity and plasticity theories, a conventional model was developed. The results from simulation were compared with those obtained from testing. The experimental data reveal that there exists certain level of uncertainty and nonlinearity in tube bending, and its variation could be significant. To overcome this, a on-line fuzzy logic controller with self-tuning capabilities was designed. The advantages of this on-line system are (1) its computational requirement is simple in comparison with more algorithmic-based controllers, and (2) the system does not need prior knowledge of material characteristics. The device includes an AC motor, a servo controller, a forming mechanism, a 3D optical sensor, and a microprocessor. This automated bending machine adopts primary and secondary errors between the actual response and desired output to conduct on-line rule reasoning. Results from testing show that the spring back angle can be effectively compensated by the self- tuning fuzzy system in a real-time fashion.

  19. Improving Linking from the Literature to On-line Data

    NASA Astrophysics Data System (ADS)

    Eichhorn, G.; Accomazzi, A.; Grant, C. S.; Henneken, E. A.; Kurtz, M. J.; Murray, S. S.

    2003-12-01

    The ADS, in close collaboration with the Astrophysics Data Centers Executive Committee (ADEC) and the American Astronomical Society (AAS) has been working on improving the linking between the literature and on-line data by allowing authors to specify data that were used in the research described in journal articles. We are working with the ADEC on identifying data sets in a consistent manner. The ADEC has agreed that all NASA data centers will use data set identifiers of the form: ADS/facility#identifier where facility specifies the telescope that acquired the data and identifier is a data center selected identifier for a particular data set. The ADS is providing a registration service for facility names that identify data collections at the various data centers, a verification service that allows authors and editors to verify the existence of data set identifiers, and a linking service that allows journals to use permanent URLs for links to data sets that may move between data centers. Current plans of the ADEC-AAS collaboration call for including data set identifiers in the LaTeX manuscripts by the authors. The data set identifiers will be provided by the data centers with all data delivered. The editorial process will verify all data set identifiers and include links to the on-line data from the on-line articles. The identifiers used in each article will be made available to the ADS for linking to the on-line data from the ADS system as well.

  20. 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…

  1. 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)

  2. 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…

  3. 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)

  4. 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]…

  5. 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…

  6. 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...

  7. On-Line IDCMS Evaluation of Different Categories of Response.

    ERIC Educational Resources Information Center

    Follettie, Joseph F.

    A manipulandum-referenced taxonomy for response categories appropriate to primary education is presented. The tenability of automatic on-line evaluation of the different types of response when processing equipment of the sort that probably will be available to Southwest Regional Laboratory is preliminarily evaluated. (Author/SK)

  8. 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…

  9. On-line mass storage system functional design document

    NASA Technical Reports Server (NTRS)

    Earnest, D.

    1975-01-01

    A functional system definition for an on-line high density magnetic tape data storage system is provided. This system can be implemented in a multi-purpose, multi-host environment, and satisfy the requirements of economical data storage in the range of 2 to 50 billion bytes.

  10. 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…