Sample records for ultra trace determination

  1. Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry.

    PubMed

    Sun, Mei; Wu, Qianghua

    2010-04-15

    A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL(-1). The relative standard deviation (n=7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin. 2009 Elsevier B.V. All rights reserved.

  2. Ultra-trace determination of plutonium in marine samples using multi-collector inductively coupled plasma mass spectrometry.

    PubMed

    Lindahl, Patric; Keith-Roach, Miranda; Worsfold, Paul; Choi, Min-Seok; Shin, Hyung-Seon; Lee, Sang-Hoon

    2010-06-25

    Sources of plutonium isotopes to the marine environment are well defined, both spatially and temporally, which makes Pu a potential tracer for oceanic processes. This paper presents the selection, optimisation and validation of a sample preparation method for the ultra-trace determination of Pu isotopes ((240)Pu and (239)Pu) in marine samples by multi-collector (MC) ICP-MS. The method was optimised for the removal of the interference from (238)U and the chemical recovery of Pu. Comparison of various separation strategies using AG1-X8, TEVA, TRU, and UTEVA resins to determine Pu in marine calcium carbonate samples is reported. A combination of anion-exchange (AG1-X8) and extraction chromatography (UTEVA/TRU) was the most suitable, with a radiochemical Pu yield of 87+/-5% and a U decontamination factor of 1.2 x 10(4). Validation of the method was accomplished by determining Pu in various IAEA certified marine reference materials. The estimated MC-ICP-MS instrumental limit of detection for (239)Pu and (240)Pu was 0.02 fg mL(-1), with an absolute limit of quantification of 0.11 fg. The proposed method allows the determination of ultra-trace Pu, at femtogram levels, in small size marine samples (e.g., 0.6-2.0 g coral or 15-20 L seawater). Finally, the analytical method was applied to determining historical records of the Pu signature in coral samples from the tropical Northwest Pacific and (239+240)Pu concentrations and (240)Pu/(239)Pu atom ratios in seawater samples as part of the 2008 GEOTRACES intercalibration exercise. Copyright 2010 Elsevier B.V. All rights reserved.

  3. Development and application of mass spectrometric techniques for ultra-trace determination of 236U in environmental samples-A review.

    PubMed

    Bu, Wenting; Zheng, Jian; Ketterer, Michael E; Hu, Sheng; Uchida, Shigeo; Wang, Xiaolin

    2017-12-01

    Measurements of the long-lived radionuclide 236 U are an important endeavor, not only in nuclear safeguards work, but also in terms of using this emerging nuclide as a tracer in chemical oceanography, hydrology, and actinide sourcing. Depending on the properties of a sample and its neutron irradiation history, 236 U/ 238 U ratios from different sources vary significantly. Therefore, this ratio can be treated as an important fingerprint for radioactive source identification, and in particular, affords a definitive means of discriminating between naturally occurring U and specific types of anthropogenic U. The development of mass spectrometric techniques makes it possible to determine ultra-trace levels of 236 U in environmental samples. In this paper, we review the current status of mass spectrometric approaches for determination of 236 U in environmental samples. Various sample preparation methods are summarized and compared. The mass spectrometric techniques emphasized herein are thermal ionization mass spectrometry (TIMS), inductively coupled plasma mass spectrometry (ICP-MS) and accelerator mass spectrometry (AMS). The strategies or principles used by each technique for the analysis of 236 U are described. The performances of these techniques in terms of abundance sensitivity and detection limit are discussed in detail. To date, AMS exhibits the best capability for ultra-trace determinations of 236 U. The levels and behaviors of 236 U in various environmental media are summarized and discussed as well. Results suggest that 236 U has an important, emerging role as a tracer for geochemical studies. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. THE CHALLENGE OF ACQUIRING ALPINE LARGE VOLUME LAKE WATER SAMPLES FOR ULTRA TRACE LEVEL ANALYSIS

    EPA Science Inventory

    The National Exposure Research Laboratory-Las Vegas, Nevada is interested in the emerging field technology of in-situ extraction of contaminants from surface water. A current research project involves ultra-trace level determination of agricultural pesticides from alpine lakes. T...

  5. Analysis of trace halocarbon contaminants in ultra high purity helium

    NASA Technical Reports Server (NTRS)

    Fewell, Larry L.

    1994-01-01

    This study describes the analysis of ultra high purity helium. Purification studies were conducted and containment removal was effected by the utilization of solid adsorbent purge-trap systems at cryogenic temperatures. Volatile organic compounds in ultra high purity helium were adsorbed on a solid adsorbent-cryogenic trap, and thermally desorbed trace halocarbon and other contaminants were analyzed by combined gas chromatography-mass spectrometry.

  6. Blood-collection device for trace and ultra-trace metal specimens evaluated.

    PubMed

    Moyer, T P; Mussmann, G V; Nixon, D E

    1991-05-01

    We evaluated the evacuated phlebotomy tube designed specifically for trace metal analysis by Sherwood Medical Co. Pools of human serum containing known concentrations of aluminum, arsenic, calcium, cadmium, copper, chromium, iron, lead, magnesium, manganese, mercury, selenium, and zinc were exposed to the tube and rubber stopper for defined periods ranging from 5 min to 24 h. Analysis for each element was performed in a randomized fashion under rigidly controlled conditions by use of standard electrothermal atomization atomic absorption spectroscopy, inductively coupled plasma atomic emission spectroscopy, and cold vapor atomic absorption spectrometry. In addition, for comparative purposes, we collected blood samples from normal volunteers by use of ultra-clean polystyrene phlebotomy syringes as well as standard evacuated phlebotomy tubes. We conclude that, except for lead, there was no significant contribution of any trace element studied from the evaluated tube and stopper to the serum. Because whole blood is the usual specimen for lead testing, the observation of a trace amount of lead in this tube designed for serum collection is trivial.

  7. Level of minerals and trace elements in the urine of the participants of mountain ultra-marathon race.

    PubMed

    Jablan, Jasna; Inić, Suzana; Stosnach, Hagen; Hadžiabdić, Maja Ortner; Vujić, Lovorka; Domijan, Ana-Marija

    2017-05-01

    The aim of the present study was to explore impact of endurance exercise on urinary level of minerals and trace elements as well as on some oxidative stress and biochemical parameters. Urine samples were collected from participants (n=21) of mountain ultra-marathon race (53km; Medvednica, Zagreb, Croatia), before (baseline value), immediately after, 12h and 24h after the race. In urine samples level of minerals (Ca, P, K and Na) and trace elements (Se, Zn, Mn, Cu, Fe and Co) were assessed using the bench top Total reflection X-ray Fluorescence (TXRF) spectrometer. Oxidative stress was determined as level of malondialdehyde (MDA). Immediately after the race level of minerals, trace elements, MDA, creatinine, ketones, erythrocytes and specific gravity increased compared to their baseline value. In 24h follow-up trace elements involved in antioxidant defence, MDA and biochemical parameters returned to their baseline values, Cu and Co remained increased as after the race, Fe and K tended to return to baseline values while Ca, P and Na continued to increase. Mountain ultra-marathon resulted in alteration of physiologically important minerals and trace elements that for some minerals and trace elements persist, indicating their involvement in recovery processes. However, due to their loss in urine, level of minerals and trace elements in athletes participating in endurance exercise should be monitored. Copyright © 2017 Elsevier GmbH. All rights reserved.

  8. PULSED SPLITLESS AND LARGE-VOLUME INJECTION IN CAPILLARY GAS CHROMATOGRAPHY MASS SPECTROMETRY FOR THE DETERMINATION OF ULTRA-TRACE LEVEL PESTICIDE RESIDUES

    EPA Science Inventory

    The possible presence of ultra-trace levels (sub- parts per trillion) of pesticides in pristine aquatic environments (e.g., alpine lakes) would raise questions regarding potential effects on biota. One hypothesis is that agricultural pesticides that are heavily applied in the San...

  9. Magnetic ionic liquid-based dispersive liquid-liquid microextraction technique for preconcentration and ultra-trace determination of Cd in honey.

    PubMed

    Fiorentini, Emiliano F; Escudero, Leticia B; Wuilloud, Rodolfo G

    2018-04-19

    A simple, highly efficient, batch, and centrifuge-less dispersive liquid-liquid microextraction method based on a magnetic ionic liquid (MIL-DLLME) and electrothermal atomic absorption spectrometry (ETAAS) detection was developed for ultra-trace Cd determination in honey. Initially, Cd(II) was chelated with ammonium diethyldithiophosphate (DDTP) at pH 0.5 followed by its extraction with the MIL trihexyl(tetradecyl)phosphonium tetrachloroferrate(III) ([P 6,6,6,14 ]FeCl 4 ) and acetonitrile as dispersant. The MIL phase containing the analyte was separated from the aqueous phase using only a magnet. A back-extraction procedure was applied to recover Cd from the MIL phase using diluted HNO 3 and this solution was directly injected into the graphite furnace of ETAAS instrument. An extraction efficiency of 93% and a sensitivity enhancement factor of 112 were obtained under optimal experimental conditions. The detection limit (LOD) was 0.4 ng L -1 Cd, while the relative standard deviation (RSD) was 3.8% (at 2 μg L -1 Cd and n = 10), calculated from the peak height of absorbance signals. This work reports the first application of the MIL [P 6,6,6,14 ]FeCl 4 along with the DLLME technique for the successful determination of Cd at trace levels in different honey samples. Graphical abstract Preconcentration of ultratraces of Cd in honey using a magnetic ionic liquid and dispersive liquid-liquid microextraction technique.

  10. Determination of ultra-trace formaldehyde in air using ammonium sulfate as derivatization reagent and capillary electrophoresis coupled with on-line electrochemiluminescence detection.

    PubMed

    Deng, Biyang; Liu, Yang; Yin, Huihui; Ning, Xi; Lu, Hua; Ye, Li; Xu, Quanxiu

    2012-03-15

    The reaction between formaldehyde and ammonium ion to produce hexamethylenetetramine is well known. The reaction conditions are very easily controlled in situ and the experiment operation is very simple. However, such derivatization reaction for trace formaldehyde determination using capillary electrophoresis (CE) electrochemiluminescence (ECL) has not been reported before. In this study, the application of ammoniun sulfate as derivatization reagent to in-situ determination of formaldehyde in air was reported. Based on ECL enhancement of tris(2,2'-bipyridyl)ruthenium(II) with hexamethylenetetramine, a novel approach for the determination of ultra-trace formaldehyde in air using CE coupled with on-line ECL of tris(2,2'-bipyridyl)ruthenium(II) has been developed. The parameters affecting separation and detection such as detection potential, concentration and pH of phosphate buffer, and electrokinetic voltage, were investigated. Under the optimal conditions, the linear concentration range of formaldehyde in air was from 0.48 μg/m(3) to 96 mg/m(3) (linear range covering 5 orders of magnitude). The limit of detection (3σ) was 0.15 μg/m(3). The relative standard deviations of peak height and migration time for six consecutive injection of 1 ng/mL formaldehyde derivative were 0.9% and 0.8%, respectively. The recoveries of formaldehyde in air were between 99.3% and 101%. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Trace matrix solid phase dispersion using a molecular sieve as the sorbent for the determination of flavonoids in fruit peels by ultra-performance liquid chromatography.

    PubMed

    Cao, Wan; Hu, Shuai-Shuai; Ye, Li-Hong; Cao, Jun; Pang, Xiao-Qing; Xu, Jing-Jing

    2016-01-01

    A simple, rapid, and highly selective trace matrix solid phase dispersion (MSPD) technique, coupled with ultra-performance liquid chromatography-ultraviolet detection, was proposed for extracting flavonoids from orange fruit peel matrices. Molecular sieve SBA-15 was applied for the first time as a solid support in trace MSPD. Parameters, such as the type of dispersant, mass ratio of the sample to the dispersant, grinding time, and elution pH, were optimized in detail. The optimal extraction conditions involved dispersing a powdered fruit peel sample (25 mg) into 25mg of SBA-15 and then eluting the target analytes with 500 μL of methanol. A satisfactory linearity (r(2) > 0.9990) was obtained, and the calculated limits of detection reached 0.02-0.03 μg/mL for the compounds. The results showed that the method developed was successfully applied to determine the content of flavonoids in complex fruit peel matrices. Copyright © 2015 Elsevier Ltd. All rights reserved.

  12. SPECTROPHOTOMETRIC DETERMINATION OF ULTRA-SMALL QUANTITIES OF NICKEL IN INDIUM (in Russian)

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

    Peshkova, V.M.; Bochkova, V.M.; Astakhova, E.K.

    1961-09-01

    alpha -Benzil doxime permits the determination of nickel by measuring optical density in the region of maximum absortption (at 275 m mu ), after the reagent excess is removed by washing the extract with alkali. Conditions were found for the spectrophotometric determination of ultra-small quantities (down to 0.005 gamma ) of nickel with alpha -benzil dioxime in the soultion of its pure salt, in the presence of cobalt and copper. A method was developed for the determination of traces of nickel down to 5 x 10 /sup -7%/ in metallic indium. The reproducibility of method is +25%. (auth)

  13. Considerations on ultra-trace analysis of phthalates in drinking water.

    PubMed

    Serôdio, P; Nogueira, J M F

    2006-07-01

    Stir bar sorptive extraction with liquid desorption followed by large volume injection and capillary gas chromatography coupled to mass spectrometry (SBSE-LD/LVI-GC-MS), had been applied for the determination of ultra-traces of seven-phthalates (dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, butyl benzyl phthalate, bis(2-ethylhexyl) adipate, bis(2-ethylhexyl) phthalate and bis(1-octyl) phthalate) in drinking water samples, which are included in the priority lists set by several international regulatory organizations. Instrumental calibration under the selected-ion monitoring mode acquisition (LVI-GC-MS(SIM)), experimental parameters that could affect the SBSE-LD efficiency, as well as, the control of the contamination profile are fully discussed. Throughout systematic assays on 30 mL water samples spiked at the 0.40 microg/L level, it had been established that stir bars coated with 47 microL of polydimethylsiloxane, an equilibrium time of 60 min (1,000 rpm) and methanol as back extraction solvent, allowed the best analytical performance to monitor phthalates in water matrices. From the data obtained, good accuracy and a remarkable reproducibility (< 14.8%) were attained, providing experimental recovery data in agreement with the theoretical equilibrium described by the octanol-water partition coefficients (K(PDMS/W) approximately K(O/W)), with the exception of bis(2-ethylhexyl) adipate, bis(2-ethylhexyl) phthalate and bis(1-octyl) phthalate, for which lower yields were measured. Additionally, a remarkable linear dynamic range between 25 and 2,000 ng/L (r(2)>0.99) and low detection limits (3-40 ng/L) were also achieved for the seven-phthalates studied. The application of the present method to monitor phthalates in tap and bottled mineral water samples, allowed convenient selectivity and high sensitivity up to 1.0 microg/L level, using the standard addition methodology. The proposed method showed to be feasible and sensitive with a low sample volume

  14. Flotation-separation and ICP-AES determination of ultra trace amounts of copper, cadmium, nickel and cobalt using 2-aminocyclopentene-1-dithiocarboxylic acid.

    PubMed

    Shamsipur, Mojtaba; Hashemi, Omid Reza; Safavi, Afsaneh

    2005-09-01

    A rapid flotation method for separation and enrichment of ultra trace amounts of copper(II), cadmium(II), nickel(II) and cobalt(II) ions from water samples is established. At pH 6.5 and with sodium dodecylsulfate used as a foaming reagent, Cu2+, Cd2+, Ni2+ and Co2+ were separated simultaneously with 2-aminocyclopentene-1-dithiocarboxylic acid (ACDA) added to 1 l of aqueous solution. The proposed procedure of preconcentration is applied prior to the determination of these four analytes using inductivity coupled plasma-atomic emission spectrometry (ICP-AES). The effects of pH, concentration of ACDA, applicability of different surfactants and foreign ions on the separation efficiency were investigated. The preconcentration factor of the method is 1000 and the detection limits of copper(II), cadmium(II), nickel(II) and cobalt(II) ions are 0.078, 0.075, 0.072 and 0.080 ng ml(-1), respectively.

  15. Application of l-cystine modified zeolite for preconcentration and determination of ultra-trace levels of cadmium by flame atomic absorption spectrometry.

    PubMed

    Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

    2016-03-04

    A very convenient, sensitive and precise solid phase extraction (SPE) system was developed for enrichment and determination of ultra-trace of cadmium ion in water and plant samples. This method was based on the retention of cadmium(II) ions by l-cystine adsorbed in Y-zeolite and carry out in a packed mini-column. The retained cadmium ions then were eluted and determined by flame atomic absorption spectrometry. The scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy techniques were applied for the characterization of cystine modified zeolite (CMZ). Some experimental conditions affecting the analytical performance such as pH, eluent type, concentration of sample, eluent flow rate and also the presence of interfering ions were investigated. The calibration graph was linear within the range of 0.1-7.5ngmL(-1) and limit of detection was obtained 0.04ngmL(-1) with the preconcentration factor of 400. The relative standard deviation (RSD) was obtained 1.4%, indicating the excellent reproducibility of this method. The proposed method was successfully applied for the extraction and determination of cadmium(II) ion in black tea, cigarette's tobacco and also various water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Surface Cleaning Techniques: Ultra-Trace ICP-MS Sample Preparation and Assay of HDPE

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

    Overman, Nicole R.; Hoppe, Eric W.; Addleman, Raymond S.

    2013-06-01

    The world’s most sensitive radiation detection and assay systems depend upon ultra-low background (ULB) materials to reduce unwanted radiological backgrounds. Herein, we evaluate methods to clean HDPE, a material of interest to ULB systems and the means to provide rapid assay of surface and bulk contamination. ULB level material and ultra-trace level detection of actinide elements is difficult to attain, due to the introduction of contamination from sample preparation equipment such as pipette tips, sample vials, forceps, etc. and airborne particulate. To date, literature available on the cleaning of such polymeric materials and equipment for ULB applications and ultra-trace analysesmore » is limited. For these reasons, a study has been performed to identify an effective way to remove surface contamination from polymers in an effort to provide improved instrumental detection limits. Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) was utilized to assess the effectiveness of a variety of leachate solutions for removal of inorganic uranium and thorium surface contamination from polymers, specifically high density polyethylene (HDPE). HDPE leaching procedures were tested to optimize contaminant removal of thorium and uranium. Calibration curves for thorium and uranium ranged from 15 ppq (fg/mL) to 1 ppt (pg/mL). Detection limits were calculated at 6 ppq for uranium and 7 ppq for thorium. Results showed the most effective leaching reagent to be clean 6 M nitric acid for 72 hour exposures. Contamination levels for uranium and thorium found in the leachate solutions were significant for ultralow level radiation detection applications.« less

  17. Optical molecular fluorescence determination of ultra-trace beryllium in occupational and environmental samples using highly alkaline conditions.

    PubMed

    Adams, Lori; Agrawal, Anoop; Cronin, John P; Ashley, Kevin

    2017-01-01

    Exposures to beryllium (Be), even at extremely low levels, can cause severe health effects in a percentage of those exposed; consequently, occupational exposure limits (OELs) promulgated for this element are the lowest established for any element. This work describes the advantages of using highly alkaline dye solutions for determination of Be in occupational hygiene and environmental samples by means of an optical molecular fluorescence technique after sample extraction in 1-3% (w˖w -1 ) aqueous ammonium bifluoride (NH 4 HF 2 ). Improved attributes include the ability to further enhance the detection limits of Be in extraction solutions of high acidity with minimal dilution, which is particularly beneficial when NH 4 HF 2 solutions of higher concentration are used for extraction of Be from soil samples. Significant improvements in Be method detection limits (MDLs) are obtained at levels many-fold below those reported previously for this methodology. Notably, MDLs for Be of <0.01 ng l -1 / 0.1 ng per sample have been attained, which are superior to MDLs routinely reported for this element by means of the most widely used ultra-trace elemental measurement technique, inductively coupled plasma mass spectrometry (ICP-MS). Very low MDLs for Be are essential in consideration of reductions in OELs for this element in workplace air by health organizations and regulatory agencies in the USA and internationally. Applications of enhanced Be measurements to air filter samples, surface wipe samples, soils and newly-designed occupational air sampler inserts are illustrated.

  18. Determination of Ultra-trace Rhodium in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction Using 2-(5-Iodo-2-Pyridylazo)-5-Dimethylaminoaniline as a Chelating Agent.

    PubMed

    Han, Quan; Huo, Yanyan; Wu, Jiangyan; He, Yaping; Yang, Xiaohui; Yang, Longhu

    2017-03-24

    A highly sensitive method based on cloud point extraction (CPE) separation/preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection has been developed for the determination of ultra-trace amounts of rhodium in water samples. A new reagent, 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA), was used as the chelating agent and the nonionic surfactant TritonX-114 was chosen as extractant. In a HAc-NaAc buffer solution at pH 5.5, Rh(III) reacts with 5-I-PADMA to form a stable chelate by heating in a boiling water bath for 10 min. Subsequently, the chelate is extracted into the surfactant phase and separated from bulk water. The factors affecting CPE were investigated. Under the optimized conditions, the calibration graph was linear in the range of 0.1-6.0 ng/mL, the detection limit was 0.023 ng/mL for rhodium and relative standard deviation was 3.67% ( c = 1.0 ng/mL, n = 11).The method has been applied to the determination of trace rhodium in water samples with satisfactory results.

  19. Optical molecular fluorescence determination of ultra-trace beryllium in occupational and environmental samples using highly alkaline conditions

    PubMed Central

    Adams, Lori; Agrawal, Anoop; Cronin, John P.; Ashley, Kevin

    2017-01-01

    Exposures to beryllium (Be), even at extremely low levels, can cause severe health effects in a percentage of those exposed; consequently, occupational exposure limits (OELs) promulgated for this element are the lowest established for any element. This work describes the advantages of using highly alkaline dye solutions for determination of Be in occupational hygiene and environmental samples by means of an optical molecular fluorescence technique after sample extraction in 1–3% (w˖w−1) aqueous ammonium bifluoride (NH4HF2). Improved attributes include the ability to further enhance the detection limits of Be in extraction solutions of high acidity with minimal dilution, which is particularly beneficial when NH4HF2 solutions of higher concentration are used for extraction of Be from soil samples. Significant improvements in Be method detection limits (MDLs) are obtained at levels many-fold below those reported previously for this methodology. Notably, MDLs for Be of <0.01 ng l−1 / 0.1 ng per sample have been attained, which are superior to MDLs routinely reported for this element by means of the most widely used ultra-trace elemental measurement technique, inductively coupled plasma mass spectrometry (ICP-MS). Very low MDLs for Be are essential in consideration of reductions in OELs for this element in workplace air by health organizations and regulatory agencies in the USA and internationally. Applications of enhanced Be measurements to air filter samples, surface wipe samples, soils and newly-designed occupational air sampler inserts are illustrated. PMID:28626294

  20. Use of an ultra-clean sampling technique with inductively coupled plasma-mass spectrometry to determine trace-element concentrations in water from the Kirkwood-Cohansey Aquifer system, coastal plain, New Jersey

    USGS Publications Warehouse

    Ivahnenko, Tamara; Szabo, Zoltan; Hall, G.S.

    1996-01-01

    Water samples were collected during 1993 from 22 public supply wells screened in the Kirkwood-Cohansey aquifer system; concentrations of 18 trace elements were determined primarily by using inductively coupled plasma-mass spectrometry (ICP-MS) techniques, though graphite furnace atomic adsorption, hydride generation, and cold- vapor flameless atomic adsorption techniques were used for thallium, arsenic, and mercury, respectively, at the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL). In addition, laboratory measurements of alkalinity and turbidity were made. The ground-water samples were collected by using ultra-clean sampling protocols developed by the USGS for collecting ground-water samples in areas with water containing low concentrations of trace elements. This technique is based on recently gained experience in sampling surface water for these elements. Field parameters (water temperature, specific conductance, pH, and dissolved-oxygen concentration) were monitored prior to sample collection. Three equipment blanks were collected to ensure that low-level trace-element contamination did not occur during sample collection. One split sample and a commercially- prepared reference standard were submitted to the NWQL o evaluate laboratory precision and accuracy, respectively. Trace-element concentrations in 10 sample splits and one equipment blank were also determined at the Rutgers University Chemistry Department laboratory. Results of the ICP-MS analyses and cold vapor flameless atomic absorption indicated that five trace elements-- cobalt, copper, lead, mercury, and nickel--were detectable in low concentrations (<0.1-29 mg/L) in most of the samples from the 22 wells, and four elements--aluminum, barium, manganese and zinc--were detected in higher concentrations than the other elements (30-710 mg/L for aluminum; 4-180 mg/L for barium, manganese, and zinc). The remaining nine trace elements were present in concentrations consistently lower

  1. Ultra-trace determination of Persistent Organic Pollutants in Arctic ice using stir bar sorptive extraction and gas chromatography coupled to mass spectrometry.

    PubMed

    Lacorte, S; Quintana, J; Tauler, R; Ventura, F; Tovar-Sánchez, A; Duarte, C M

    2009-12-04

    This study presents the optimization and application of an analytical method based on the use of stir bar sorptive extraction (SBSE) gas chromatography coupled to mass spectrometry (GC-MS) for the ultra-trace analysis of POPs (Persistent Organic Pollutants) in Arctic ice. In a first step, the mass-spectrometry conditions were optimized to quantify 48 compounds (polycyclic aromatic hydrocarbons, brominated diphenyl ethers, chlorinated biphenyls, and organochlorinated pesticides) at the low pg/L level. In a second step, the performance of this analytical method was evaluated to determine POPs in Arctic cores collected during an oceanographic campaign. Using a calibration range from 1 to 1800 pg/L and by adjusting acquisition parameters, limits of detection at the 0.1-99 and 102-891 pg/L for organohalogenated compounds and polycyclic aromatic hydrocarbons, respectively, were obtained by extracting 200 mL of unfiltered ice water. alpha-hexachlorocyclohexane, DDTs, chlorinated biphenyl congeners 28, 101 and 118 and brominated diphenyl ethers congeners 47 and 99 were detected in ice cores at levels between 0.5 to 258 pg/L. We emphasise the advantages and disadvantages of in situ SBSE in comparison with traditional extraction techniques used to analyze POPs in ice.

  2. Gold nanochestnut arrays as ultra-sensitive SERS substrate for detecting trace pesticide residue.

    PubMed

    Geng, Fei; Zhao, Huaping; Fu, Qun; Mi, Yan; Miao, Likun; Li, Wei; Dong, Yulian; Wu, Minghong; Lei, Yong

    2018-07-20

    In comparison to conventional spectroscopic techniques based on chromatography, surface-enhanced Raman spectroscopy (SERS) enables the rapid identification and detection of trace pesticide residues present in trace amounts in the environment and foods. Herein, a facile approach to fabricate unique gold nanochestnuts (GNCs) as an ultra-sensitive SERS substrate for detecting trace pesticide residues has been developed based on anodic aluminum oxide (AAO) templates. The GNCs are synthesized through the galvanic replacement of Ag on the top of Ni nanorod arrays. The as-prepared GNCs have well-controlled structural parameters, and importantly have unique anisotropic morphologies that benefit the enhancement in SERS performance. As a result, rhodamine 6 G (R6G) can be efficiently detected with GNCs as the SERS substrate even with a concentration of only 10 -12 M, and the Raman enhancement factor reaches up to 5.4 × 10 9 at this concentration. Further SERS measurement of thiram indicates a remarkable SERS-active sensitivity of the as-prepared GNCs with a detection limit of thiram up to 10 -14 M. The GNCs also exhibit a high signal-to-noise ratio.

  3. Preconcentration and speciation of ultra-trace Se (IV) and Se (VI) in environmental water samples with nano-sized TiO2 colloid and determination by HG-AFS.

    PubMed

    Fu, Jiaqi; Zhang, Xu; Qian, Shahua; Zhang, Lin

    2012-05-30

    A united method for speciation analysis of Se (IV) and Se (VI) in environmental water samples was developed using nano-sized TiO(2) colloid as adsorbent and hydride generation atomic fluorescence spectrometry (HG-AFS) as determination means. When the pH values of bulk solution were between 6.0 and 7.0, successful adsorption onto 1 mL nano-sized TiO(2) colloid (0.2%) was achieved for more than 97.0% of Se (IV) while Se (VI) barely got adsorbed. Therefore, the method made it possible to preconcentrate and determine Se (IV) and Se (VI) separately. The precipitated TiO(2) with concentrated selenium was directly converted to colloid without desorption. Selenium in the resulting colloid was then determined by HG-AFS. The detection limits (3σ) and relative standard deviations (R.S.D) of this method were 24 ng/L and 42 ng/L, 7.8% (n=6) and 7.0% (n=6) for Se (IV) and Se (VI), respectively. This simple, sensitive, and united method was successfully applied to the separation and speciation of ultra-trace Se (IV) and Se (VI) in environmental water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Simultaneous trace multielement determination by ICP-OES after solid phase extraction with modified octadecyl silica gel.

    PubMed

    Karbasi, Mohamad-Hadi; Jahanparast, Babak; Shamsipur, Mojtaba; Hassan, Jalal

    2009-10-15

    Multielement simultaneous determination of 35 trace elements in environmental samples was carried out by inductively coupled plasma emission spectrometry (ICP-OES) after preconcentration with octadecyl silicagel, modified with aurin tricarboxylic acid (Aluminon). Optimal experimental conditions including pH of sample solution, sample volume, sample and eluent flow rate, type, concentration and volume of eluent and foreign ions effect were investigated and established. Trace element ions in aqueous solution were quantitatively adsorbed onto octadecyl silicagel modified with aurin tricarboxylic acid at pH 8.0 with a flow rate of 11.0 mL min(-1). The adsorbed element ions were eluted with 3-5 mL of 0.5 mol L(-1) HNO(3) at a flow rate of 10.0 mL min(-1) and analyzed by ICP-OES simultaneously. The proposed method has at least preconcentration factor of 100 in water samples, which results high sensitive detection of ultra-trace and trace analysis. The present methodology gave recoveries better than 70% and RSD less than 16%.

  5. Novel electrochemical biosensor based on PVP capped CoFe2O4@CdSe core-shell nanoparticles modified electrode for ultra-trace level determination of rifampicin by square wave adsorptive stripping voltammetry.

    PubMed

    Asadpour-Zeynali, Karim; Mollarasouli, Fariba

    2017-06-15

    This work introduces a new electrochemical sensor based on polyvinyl pyrrolidone capped CoFe 2 O 4 @CdSe core-shell modified electrode for a rapid detection and highly sensitive determination of rifampicin (RIF) by square wave adsorptive stripping voltammetry. The new PVP capped CoFe 2 O 4 @CdSe with core-shell nanostructure was synthesized by a facile synthesis method for the first time. PVP can act as a capping and etching agent for protection of the outer surface nanoparticles and formation of a mesoporous shell, respectively. Another important feature of this work is the choice of the ligand (1,10-phenanthroline) for precursor cadmium complex that works as a chelating agent in order to increase optical and electrical properties and stability of prepared nanomaterial. The nanoparticles have been characterized by field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), UV-vis, photoluminescence (PL) spectroscopy, FT-IR, and cyclic voltammetry techniques. The PL spectroscopy study of CoFe 2 O 4 @CdSe has shown significant PL quenching by the formation of CoFe 2 O 4 core inside CdSe, this shows that CoFe 2 O 4 NPs are efficient electron acceptors with the CdSe. It is clearly observed that the biosensor can significantly enhance electrocatalytic activity towards the oxidation of RIF, under the optimal conditions. The novelty of this work arises from the new synthesis method for the core-shell of CoFe 2 O 4 @CdSe. Then, the novel electrochemical biosensor was fabricated for ultra-trace level determination of rifampicin with very low detection limit (4.55×10 -17 M) and a wide linear range from 1.0×10 -16 to 1.0×10 -7 M. The fabricated biosensor showed high sensitivity and selectivity, good reproducibility and stability. Therefore, it was successfully applied for the determination of ultra-trace RIF amounts in biological and pharmaceutical samples with

  6. Ultra-rapid EOP determination with VLBI

    NASA Astrophysics Data System (ADS)

    Haas, Rüdiger; Kurihara, Shinobu; Nozawa, Kentaro; Hobiger, Thomas; Lovell, Jim; McCallum, Jamie; Quick, Jonathan

    2013-04-01

    In 2007 the Geospatial information Authority of Japan (GSI) and the Onsala Space Observatory (OSO) started a project aiming at determining the earth rotation angle, usually expressed as dUT1, in near real-time. In the beginning of this project dedicated one hour long one-baseline experiments were observed periodically using the VLBI stations Onsala (Sweden) and Tsukuba (Japan). The strategy is that the observed VLBI-data are sent in real-time via the international optical fibre backbone to the VLBI-correlator at Tsukuba where the data are correlated and analyzed in near-real time, producing ultra-rapid dUT1 results. An offline version of this strategy has been adopted in 2009 for the regular VLBI intensive series INT-2 involving Wettzell (Germany) and Tsukuba. Since March 2010 the INT-2 is using real-time e-transfer, too, and since June 2010 also automated analysis. Starting in 2009 the ultra-rapid approach was applied to regular 24 hour long VLBI-sessions that involve Tsukuba and Onsala, so that ultra-rapid dUT1 results can be produced already during ongoing VLBI-sessions. This strategy was successfully operated during the 15 days long CONT11 campaign. In 2011 the ultra-rapid strategy was extended to involve a network of VLBI-stations, so that not only dUT1 but also the polar motion components can be determined in near real-time. Initially, in November 2011 a dedicated three-station session was observed involving Onsala, Tsukuba and Hobart (Tasmania, Australia). In 2012 several regular 24 hour long IVS-sessions that involved Onsala, Tsukuba and HartRAO (South Africa) were operated with the ultra-rapid strategy, and in several cases also Hobart was added as a fourth station. For this project we use the new analysis software c5++ developed by the National Institute of Information and Communications Technology (NICT). In this presentation we give an overview of the UREOP-project, describe the recent developments, and discuss the obtained results.

  7. Enantioselective column coupled electrophoresis employing large bore capillaries hyphenated with tandem mass spectrometry for ultra-trace determination of chiral compounds in complex real samples.

    PubMed

    Piešťanský, Juraj; Maráková, Katarína; Kovaľ, Marián; Havránek, Emil; Mikuš, Peter

    2015-12-01

    A new multidimensional analytical approach for the ultra-trace determination of target chiral compounds in unpretreated complex real samples was developed in this work. The proposed analytical system provided high orthogonality due to on-line combination of three different methods (separation mechanisms), i.e. (1) isotachophoresis (ITP), (2) chiral capillary zone electrophoresis (chiral CZE), and (3) triple quadrupole mass spectrometry (QqQ MS). The ITP step, performed in a large bore capillary (800 μm), was utilized for the effective sample pretreatment (preconcentration and matrix clean-up) in a large injection volume (1-10 μL) enabling to obtain as low as ca. 80 pg/mL limits of detection for the target enantiomers in urine matrices. In the chiral CZE step, the different chiral selectors (neutral, ionizable, and permanently charged cyclodextrins) and buffer systems were tested in terms of enantioselectivity and influence on the MS detection response. The performance parameters of the optimized ITP - chiral CZE-QqQ MS method were evaluated according to the FDA guidance for bioanalytical method validation. Successful validation and application (enantioselective monitoring of renally eliminated pheniramine and its metabolite in human urine) highlighted great potential of this chiral approach in advanced enantioselective biomedical applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. A sensitive flow-batch system for on board determination of ultra-trace ammonium in seawater: Method development and shipboard application.

    PubMed

    Zhu, Yong; Yuan, Dongxing; Huang, Yongming; Ma, Jian; Feng, Sichao

    2013-09-10

    Combining fluorescence detection with flow analysis and solid phase extraction (SPE), a highly sensitive and automatic flow system for measurement of ultra-trace ammonium in open ocean water was established. Determination was based on fluorescence detection of a typical product of o-phthaldialdehyde and ammonium. In this study, the fluorescence reaction product could be efficiently extracted onto an SPE cartridge (HLB, hydrophilic-lipophilic balance). The extracted fluorescence compounds were rapidly eluted with ethanol and directed into a flow cell for fluorescence detection. Compared with the common used fluorescence method, the proposed one offered the benefits of improved sensitivity, reduced reagent consumption, negligible salinity effect and lower cost. Experimental parameters were optimized using a univariate experimental design. Calibration curves, ranging from 1.67 to 300nM, were obtained with different reaction times. The recoveries were between 89.5 and 96.5%, and the detection limits in land-based and shipboard laboratories were 0.7 and 1.2nM, respectively. The relative standard deviation was 3.5% (n=5) for an aged seawater sample spiked with 20nM ammonium. Compared with the analytical results obtained using the indophenol blue method coupled to a long-path liquid waveguide capillary cell, the proposed method showed good agreement. The method had been applied on board during a South China Sea cruise in August 2012. A vertical profile of ammonium in the South East Asia Time-Series (SEATS, 18° N, 116° E) station was produced. The distribution of ammonium in the surface seawater of the Qiongdong upwelling in South China Sea is also presented. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

    PubMed

    Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

    2013-12-15

    A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. SMUVS: Spitzer Matching survey of the UltraVISTA ultra-deep Stripes

    NASA Astrophysics Data System (ADS)

    Caputi, Karina; Ashby, Matthew; Fazio, Giovanni; Huang, Jiasheng; Dunlop, James; Franx, Marijn; Le Fevre, Olivier; Fynbo, Johan; McCracken, Henry; Milvang-Jensen, Bo; Muzzin, Adam; Ilbert, Olivier; Somerville, Rachel; Wechsler, Risa; Behroozi, Peter; Lu, Yu

    2014-12-01

    We request 2026.5 hours to homogenize the matching ultra-deep IRAC data of the UltraVISTA ultra-deep stripes, producing a final area of ~0.6 square degrees with the deepest near- and mid-IR coverage existing in any such large area of the sky (H, Ks, [3.6], [4.5] ~ 25.3-26.1 AB mag; 5 sigma). The UltraVISTA ultra-deep stripes are contained within the larger COSMOS field, which has a rich collection of multi-wavelength, ancillary data, making it ideal to study different aspects of galaxy evolution with high statistical significance and excellent redshift accuracy. The UltraVISTA ultra-deep stripes are the region of the COSMOS field where these studies can be pushed to the highest redshifts, but securely identifying high-z galaxies, and determining their stellar masses, will only be possible if ultra-deep mid-IR data are available. Our IRAC observations will allow us to: 1) extend the galaxy stellar mass function at redshifts z=3 to z=5 to the intermediate mass regime (M~5x10^9-10^10 Msun), which is critical to constrain galaxy formation models; 2) gain a factor of six in the area where it is possible to effectively search for z>=6 galaxies and study their properties; 3) measure, for the first time, the large-scale structure traced by an unbiased galaxy sample at z=5 to z=7, and make the link to their host dark matter haloes. This cannot be done in any other field of the sky, as the UltraVISTA ultra-deep stripes form a quasi-contiguous, regular-shape field, which has a unique combination of large area and photometric depth. 4) provide a unique resource for the selection of secure z>5 targets for JWST and ALMA follow up. Our observations will have an enormous legacy value which amply justifies this new observing-time investment in the COSMOS field. Spitzer cannot miss this unique opportunity to open up a large 0.6 square-degree window to the early Universe.

  11. Ultra-trace analysis of hormones, pharmaceutical substances, alkylphenols and phthalates in two French natural mineral waters.

    PubMed

    Dévier, Marie-Hélène; Le Menach, Karyn; Viglino, Liza; Di Gioia, Lodovico; Lachassagne, Patrick; Budzinski, Hélène

    2013-01-15

    The aim of this work was to investigate the potential presence of a broad range of organic compounds, such as hormones, alkylphenols, bisphenol A and phthalates, as well as pharmaceutical substances in two brands of bottled natural mineral waters (Evian and Volvic, Danone). The phthalates were determined by solid-phase microextraction coupled to gas chromatography-mass spectrometry (SPME-GC-MS) and the other compounds by liquid chromatography-tandem mass spectrometry (LC-MS/MS) or gas chromatography-mass spectrometry (GC-MS) after solid-phase extraction. The potential migration of alkylphenols, bisphenol A and phthalates from polyethylene terephthalate (PET) bottles was also investigated under standardized test conditions. Evian and Volvic natural mineral waters contain none of the around 120 targeted organic compounds. Traces of 3 pharmaceuticals (ketoprofen, salicylic acid, and caffeine), 3 alkylphenols (4-nonylphenol, 4-t-octylphenol, and 4-nonylphenol diethoxylate), and some phthalates including di(2-ethylhexyl)phthalate (DEHP) were detected in the samples, but they were also present in the procedural blanks at similar levels. The additional test procedures demonstrated that the few detected compounds originated from the background laboratory contamination. Analytical procedures have been designed both in the bottling factory and in the laboratory in order to investigate the sources of DEHP and to minimize to the maximum this unavoidable laboratory contamination. It was evidenced that no migration of the targeted compounds from bottles occurred under the test conditions. The results obtained in this study underline the complexity of reaching a reliable measure to qualify the contamination of a sample at ultra-trace level, in the field of very pure matrices. The analytical procedures involving glassware, equipment, hoods, and rooms specifically dedicated to trace analysis allowed us to reach reliable procedural limits of quantification at the ng/L level, by

  12. The effect of acidified sample storage time on the determination of trace element concentration in ice cores by ICP-SFMS

    NASA Astrophysics Data System (ADS)

    Uglietti, C.; Gabrielli, P.; Lutton, A.; Olesik, J.; Thompson, L. G.

    2012-12-01

    Trace elements in micro-particles entrapped in ice cores are a valuable proxy of past climate and environmental variations. Inductively coupled plasma sector field mass spectrometry (ICP-SFMS) is generally recognized as a sensitive and accurate technique for the quantification of ultra-trace element concentrations in ice cores. Usually, ICP-SFMS analyses of ice core samples are performed by melting and acidifying aliquots. Acidification is important to transfer trace elements from particles into solution by partial and/or complete dissolution. Only elements in solution and in sufficiently small particles will be vaporized and converted to elemental ions in the plasma for detection by ICP-SFMS. However, experimental results indicate that differences in acidified sample storage time at room temperature may lead to the recovery of different trace element fractions. Moreover, different lithologies of the relatively abundant crustal material entrapped in the ice matrix could also influence the fraction of trace elements that are converted into elemental ions in the plasma. These factors might affect the determination of trace elements concentrations in ice core samples and hamper the comparison of results obtained from ice cores from different locations and/or epochs. In order to monitor the transfer of elements from particles into solution in acidified melted ice core samples during storage, a test was performed on sections from nine ice cores retrieved from low latitude drilling sites around the world. When compared to ice cores from polar regions, these samples are characterized by a relative high content of micro-particles that may leach trace elements into solution differently. Of the nine ice cores, five are from the Tibetan Plateau (Dasuopu, Guliya, Naimonanyi, Puruogangri and Dunde), two from the Andes (Quelccaya and Huascaran), one from Africa (Kilimanjaro) and one from the Eastern Alps (Ortles). These samples were decontaminated by triple rinsing, melted and

  13. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry

    NASA Astrophysics Data System (ADS)

    Amin, Alaa S.; El-Sharjawy, Abdel-Azeem M.; Kassem, Mohammed A.

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L-1 of Tl(III) with relative standard deviation (RSD) of 1.40% (n = 10). The detection and quantification limits are 150 and 495 ng L-1 using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31 × 107 L mol-1 cm-1 and 0.00156 ng cm-2, respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples.

  14. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry.

    PubMed

    Amin, Alaa S; El-Sharjawy, Abdel-Azeem M; Kassem, Mohammed A

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L(-1) of Tl(III) with relative standard deviation (RSD) of 1.40% (n=10). The detection and quantification limits are 150 and 495 ng L(-1) using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31×10(7) L mol(-1)cm(-1) and 0.00156 ng cm(-2), respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. INAA Application for Trace Element Determination in Biological Reference Material

    NASA Astrophysics Data System (ADS)

    Atmodjo, D. P. D.; Kurniawati, S.; Lestiani, D. D.; Adventini, N.

    2017-06-01

    Trace element determination in biological samples is often used in the study of health and toxicology. Determination change to its essentiality and toxicity of trace element require an accurate determination method, which implies that a good Quality Control (QC) procedure should be performed. In this study, QC for trace element determination in biological samples was applied by analyzing the Standard Reference Material (SRM) Bovine muscle 8414 NIST using Instrumental Neutron Activation Analysis (INAA). Three selected trace element such as Fe, Zn, and Se were determined. Accuracy of the elements showed as %recovery and precision as %coefficient of variance (%CV). The result showed that %recovery of Fe, Zn, and Se were in the range between 99.4-107%, 92.7-103%, and 91.9-112%, respectively, whereas %CV were 2.92, 3.70, and 5.37%, respectively. These results showed that INAA method is precise and accurate for trace element determination in biological matrices.

  16. Temperature Programmed Desorption of Quench-condensed Krypton and Acetone in Air; Selective Concentration of Ultra-trace Gas Components.

    PubMed

    Suzuki, Taku T; Sakaguchi, Isao

    2016-01-01

    Selective concentration of ultra-trace components in air-like gases has an important application in analyzing volatile organic compounds in the gas. In the present study, we examined quench-condensation of the sample gas on a ZnO substrate below 50 K followed by temperature programmed desorption (TPD) (low temperature TPD) as a selective gas concentration technique. We studied two specific gases in the normal air; krypton as an inert gas and acetone as a reactive gas. We evaluated the relationship between the operating condition of low temperature TPD and the lowest detection limit. In the case of krypton, we observed the selective concentration by exposing at 6 K followed by thermal desorption at about 60 K. On the other hand, no selectivity appeared for acetone although trace acetone was successfully concentrated. This is likely due to the solvent effect by a major component in the air, which is suggested to be water. We suggest that pre-condensation to remove the water component may improve the selectivity in the trace acetone analysis by low temperature TPD.

  17. A portable fluorescence detector for fast ultra trace detection of explosive vapors

    NASA Astrophysics Data System (ADS)

    Xin, Yunhong; He, Gang; Wang, Qi; Fang, Yu

    2011-10-01

    This paper developed a portable detector based on a specific material-based fluorescent sensing film for an ultra trace detection of explosives, such as 2,4,6-trinitrotoluene (TNT) or its derivate 2,4-dinitrotoluene (DNT), in ambient air or on objects tainted by explosives. The fluorescent sensing films are based on single-layer chemistry and the signal amplification effect of conjugated polymers, which exhibited higher sensitivity and shorter response time to TNT or DNT at their vapor pressures. Due to application of the light emitting diode and the solid state photomultiplier and the cross-correlation-based circuit design technology, the device has the advantages of low-power, low-cost, small size, and an improved signal to noise ratio. The results of the experiments showed that the detector can real-time detect and identify of explosive vapors at extremely low levels; it is suitable for the identification of suspect luggage, forensic analyses, or battlefields clearing.

  18. A portable fluorescence detector for fast ultra trace detection of explosive vapors.

    PubMed

    Xin, Yunhong; He, Gang; Wang, Qi; Fang, Yu

    2011-10-01

    This paper developed a portable detector based on a specific material-based fluorescent sensing film for an ultra trace detection of explosives, such as 2,4,6-trinitrotoluene (TNT) or its derivate 2,4-dinitrotoluene (DNT), in ambient air or on objects tainted by explosives. The fluorescent sensing films are based on single-layer chemistry and the signal amplification effect of conjugated polymers, which exhibited higher sensitivity and shorter response time to TNT or DNT at their vapor pressures. Due to application of the light emitting diode and the solid state photomultiplier and the cross-correlation-based circuit design technology, the device has the advantages of low-power, low-cost, small size, and an improved signal to noise ratio. The results of the experiments showed that the detector can real-time detect and identify of explosive vapors at extremely low levels; it is suitable for the identification of suspect luggage, forensic analyses, or battlefields clearing.

  19. Major to ultra trace elements in rainfall collected in suburban Tokyo

    NASA Astrophysics Data System (ADS)

    Shimamura, Tadashi; Iwashita, Masato; Iijima, Satoe; Shintani, Megumi; Takaku, Yuichi

    Major to ultra trace elements such as rare earth elements (REEs), platinum group elements (PGEs) in 20 rainfall events from suburban Tokyo were determined by inductively coupled plasma mass spectrometry (ICP-MS). Anion species were also determined by an ion chromatography (IC). The concentrations of PGEs were so low that only Pt was detected in some rainfall events. Enrichment factors (EFs), refer to soil and sea salt components, were calculated for the measured elements (with Al and Na as references). Be, (Na), Mg, (Al), Si, Cl, K, Fe, Rb, Sr, REEs (except La, Gd), Ta, and U were mostly originated from natural materials (soil and sea salt). For Li, B, Ca, Mn, Sr, Ba, and Cs, the contribution of natural materials was significant. EFs for Cu, Zn, As, Se, Sb, Cd, Pb, Bi, Ag, Te, Au, Pt, SO 4-S and NO 3-N exceeded 100 indicating non-crustal, non-sea salt origin, presumably anthropogenic; however, contribution of volcanic gases could not be excluded for As, Se, Te and Bi. Pt seemed to be uniformly distributed worldwide and a catalyst for automobile emission control may be the main source. Au also showed uniform distribution. On the other hand, EFs for Zr, Nb, Hf and Th were less than unity. Probably these elements resided in acid resistant refractory fine minerals that did not decompose with acid treatment, and did not evaporate and ionize in the ICP. An alternative explanation is that the concentration of these elements was lower in the soil of the sampling area than the average crust. In the crust normalized REE pattern plot, La, Eu and Gd showed clear positive anomalies. La and Gd could have anthropogenic components. A possible source of La and Gd is cracking catalyst for petrol refining, but this source does not fully explain the anomaly. The source of Gd may also be Gd-DTPA (Gadolinium (III) diethyltriaminepentaacetic acid) used for Magnetic Resonance Imaging (MRI) contrast agents. The Eu origin may be soil with higher concentration than the crust average.

  20. Determination of trace levels of benzophenone-type ultra-violet filters in real matrices by bar adsorptive micro-extraction using selective sorbent phases.

    PubMed

    Almeida, C; Stępkowska, A; Alegre, A; Nogueira, J M F

    2013-10-11

    Bar adsorptive micro-extraction (BAμE), using selective sorbent phases, followed by liquid desorption in combination with high performance liquid chromatography-diode array detection (BAμE-LD/HPLC-DAD), is proposed for the determination of trace levels of four benzophenone-type UV filters (benzophenone, 2-hydroxy-4-methoxy-benzophenone, 2,4-hydroxybenzophenone and 4-hydroxybenzophenone) in real matrices. By comparing three polymers (P1, P2 and P3) and five activated carbons (AC1, AC2, AC3, AC4 and AC5) phases, P2 (a modified pyrrolidone polymer) and AC4 coatings showed much higher selectivity and capacity through BAμE, where the former offers multiple mechanisms of interaction and faster equilibrium kinetics. Assays performed on 25mL of ultra-pure water samples spiked at the 8.0μg/L level, yielded recoveries ranging from 76.6±8.3% to 103.5±6.4% depending on the sorbent phase used (P2 or AC4), under optimized experimental conditions. The analytical performance showed convenient detection limits (0.3-0.5μg/L) and good linear dynamic ranges (1.0-24.0μg/L) with remarkable determination coefficients (r(2)>0.9969). Excellent repeatability was also achieved through intraday (RSD<13.0%) and interday (RSD<8.9%) experiments. By using the standard addition methodology, the application of the present analytical approach on sea water, wastewater, commercial cosmetic products and urine samples revealed good sensitivity, absence of matrix effects and the occurrence of levels of some benzophenones. The proposed methodology that uses nanostructured particles and operates under the floating sampling technology proved to be a sorption-based static micro-extraction alternative to monitor benzophenone-type UV filters in real matrices. Moreover, is easy to implement, reliable, sensitive, requiring low sample volume and the possibility to choose the most selective sorbent coating according to the target compounds involved. Copyright © 2013. Published by Elsevier B.V.

  1. Preparation of novel alumina nanowire solid-phase microextraction fiber coating for ultra-selective determination of volatile esters and alcohols from complicated food samples.

    PubMed

    Zhang, Zhuomin; Ma, Yunjian; Wang, Qingtang; Chen, An; Pan, Zhuoyan; Li, Gongke

    2013-05-17

    A novel alumina nanowire (ANW) solid-phase microextraction (SPME) fiber coating was prepared by a simple and rapid anodization-chemical etching method for ultra-selective determination of volatile esters and alcohols from complicated food samples. Preparation conditions for ANW SPME fiber coating including corrosion solution concentration and corrosion time were optimized in detail for better surface morphology and higher surface area based on scanning electron microscope (SEM). Under the optimum conditions, homogeneous alumina nanowire structure of ANW SPME fiber coating was achieved with the average thickness of 20 μm around. Compared with most of commercial SPME fiber coatings, ANW SPME fiber coatings achieved the higher extraction capacity and special selectivity for volatile esters and alcohols. Finally, an efficient gas sampling technique based on ANW SPME fiber coating as the core was established and successfully applied for the ultra-selective determination of trace volatile esters and alcohols from complicated banana and fermented glutinous rice samples coupled with gas chromatography/mass spectrometry (GC/MS) detection. It was interesting that 25 esters and 2 alcohols among 30 banana volatile organic compounds (VOCs) identified and 4 esters and 7 alcohols among 13 identified VOCs of fermented glutinous rice were selectively sampled by ANW SPME fiber coatings. Furthermore, new analytical methods for the determination of some typical volatile esters and alcohols from banana and fermented glutinous rice samples at specific storage or brewing phases were developed and validated. Good recoveries for banana and fermented glutinous rice samples were achieved in range of 108-115% with relative standard deviations (RSDs) of 2.6-6.7% and 80.0-91.8% with RSDs of 0.3-1.3% (n=3), respectively. This work proposed a novel and efficient gas sampling technique of ANW SPME which was quite suitable for ultra-selectively sampling trace volatile esters and alcohols from

  2. Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction.

    PubMed

    Chen, YiQuan; Cheng, Xian; Mo, Fan; Huang, LiMei; Wu, Zujian; Wu, Yongning; Xu, LiangJun; Fu, FengFu

    2016-04-01

    A simple dispersive solid-phase extraction (DSPE) used to extract and preconcentrate ultra-trace MeHg, EtHg and Hg(2+) from water sample, and a sensitive method for the simultaneous analysis of MeHg, EtHg and Hg(2+) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) with field-amplified sample stacking injection (FASI) were first reported in this study. The DSPE used thiol cotton particles as adsorbent, and is simple and effective. It can be used to extract and preconcentrate ultra-trace mercury compounds in water samples within 30 min with a satisfied recovery and no mercury species alteration during the process. The FASI enhanced the sensitivity of CE-ICP-MS with 25-fold, 29-fold and 27-fold for MeHg, EtHg and Hg(2+) , respectively. Using FASI-CE-ICP-MS together with DSPE, we have successfully determined ultra-trace MeHg, EtHg and Hg(2+) in tap water with a limits of quantification (LOQs) of 0.26-0.45 pg/mL, an RSD (n = 3) < 6% and a recovery of 92-108%. Ultra-high sensitivity, as well as much less sample and reagent consumption and low operating cost, make our method a valuable technique to the speciation analysis of ultra-trace mercury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Direct analysis of ultra-trace semiconductor gas by inductively coupled plasma mass spectrometry coupled with gas to particle conversion-gas exchange technique.

    PubMed

    Ohata, Masaki; Sakurai, Hiromu; Nishiguchi, Kohei; Utani, Keisuke; Günther, Detlef

    2015-09-03

    An inductively coupled plasma mass spectrometry (ICPMS) coupled with gas to particle conversion-gas exchange technique was applied to the direct analysis of ultra-trace semiconductor gas in ambient air. The ultra-trace semiconductor gases such as arsine (AsH3) and phosphine (PH3) were converted to particles by reaction with ozone (O3) and ammonia (NH3) gases within a gas to particle conversion device (GPD). The converted particles were directly introduced and measured by ICPMS through a gas exchange device (GED), which could penetrate the particles as well as exchange to Ar from either non-reacted gases such as an air or remaining gases of O3 and NH3. The particle size distribution of converted particles was measured by scanning mobility particle sizer (SMPS) and the results supported the elucidation of particle agglomeration between the particle converted from semiconductor gas and the particle of ammonium nitrate (NH4NO3) which was produced as major particle in GPD. Stable time-resolved signals from AsH3 and PH3 in air were obtained by GPD-GED-ICPMS with continuous gas introduction; however, the slightly larger fluctuation, which could be due to the ionization fluctuation of particles in ICP, was observed compared to that of metal carbonyl gas in Ar introduced directly into ICPMS. The linear regression lines were obtained and the limits of detection (LODs) of 1.5 pL L(-1) and 2.4 nL L(-1) for AsH3 and PH3, respectively, were estimated. Since these LODs revealed sufficiently lower values than the measurement concentrations required from semiconductor industry such as 0.5 nL L(-1) and 30 nL L(-1) for AsH3 and PH3, respectively, the GPD-GED-ICPMS could be useful for direct and high sensitive analysis of ultra-trace semiconductor gas in air. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Highly selective micro-sequential injection lab-on-valve (muSI-LOV) method for the determination of ultra-trace concentrations of nickel in saline matrices using detection by electrothermal atomic absorption spectrometry.

    PubMed

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

    2006-10-01

    A highly selective procedure is proposed for the determination of ultra-trace level concentrations of nickel in saline aqueous matrices exploiting a micro-sequential injection Lab-On-Valve (muSI-LOV) sample pretreatment protocol comprising bead injection separation/pre-concentration and detection by electrothermal atomic absorption spectrometry (ETAAS). Based on the dimethylglyoxime (DMG) reaction used for nickel analysis, the sample, as contained in a pH 9.0 buffer, is, after on-line merging with the chelating reagent, transported to a reaction coil attached to one of the external ports of the LOV to assure sufficient reaction time for the formation of Ni(DMG)(2) chelate. The non-ionic coordination compound is then collected in a renewable micro-column packed with a reversed-phase copolymeric sorbent [namely, poly(divinylbenzene-co-N-vinylpyrrolidone)] containing a balanced ratio of hydrophilic and lipophilic monomers. Following elution by a 50-muL methanol plug in an air-segmented modality, the nickel is finally quantified by ETAAS. Under the optimized conditions and for a sample volume of 1.8 mL, a retention efficiency of 70 % and an enrichment factor of 25 were obtained. The proposed methodology showed a high tolerance to the commonly encountered alkaline earth matrix elements in environmental waters, that is, calcium and magnesium, and was successfully applied for the determination of nickel in an NIST standard reference material (NIST 1640-Trace elements in natural water), household tap water of high hardness and local seawater. Satisfying recoveries were achieved for all spiked environmental water samples with maximum deviations of 6 %. The experimental results for the standard reference material were not statistically different to the certified value at a significance level of 0.05.

  5. Method for determination of levoglucosan in snow and ice at trace concentration levels using ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

    PubMed

    You, Chao; Song, Lili; Xu, Baiqing; Gao, Shaopeng

    2016-02-01

    A method is developed for determination of levoglucosan at trace concentration levels in complex matrices of snow and ice samples. This method uses an injection mixture comprising acetonitrile and melt sample at a ratio of 50/50 (v/v). Samples are analyzed using ultra-performance liquid chromatography system combined with triple tandem quadrupole mass spectrometry (UPLC-MS/MS). Levoglucosan is analyzed on BEH Amide column (2.1 mm × 100 mm, 1.7 um), and a Z-spray electrospray ionization source is used for levoglucosan ionization. The polyether sulfone filter is selected for filtrating insoluble particles due to less impact on levoglucosan. The matrix effect is evaluated by using a standard addition method. During the method validation, limit of detection (LOD), linearity, recovery, repeatability and reproducibility were evaluated using standard addition method. The LOD of this method is 0.11 ng mL(-1). Recoveries vary from 91.2% at 0.82 ng mL(-1) to 99.3% at 4.14 ng mL(-1). Repeatability ranges from 17.9% at a concentration of 0.82 ng mL(-1) to 2.8% at 4.14 ng mL(-1). Reproducibility ranges from 15.1% at a concentration of 0.82 ng mL(-1) to 1.9% at 4.14 ng mL(-1). This method can be implemented using less than 0.50 mL sample volume in low and middle latitude regions like the Tibetan Plateau. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Comparison of methods for measurement of organic compounds at ultra-trace level: analytical criteria and application to analysis of amino acids in extraterrestrial samples.

    PubMed

    Vandenabeele-Trambouze, O; Claeys-Bruno, M; Dobrijevic, M; Rodier, C; Borruat, G; Commeyras, A; Garrelly, L

    2005-02-01

    The need for criteria to compare different analytical methods for measuring extraterrestrial organic matter at ultra-trace levels in relatively small and unique samples (e.g., fragments of meteorites, micrometeorites, planetary samples) is discussed. We emphasize the need to standardize the description of future analyses, and take the first step toward a proposed international laboratory network for performance testing.

  7. Chemical Sensing for Buried Landmines - Fundamental Processes Influencing Trace Chemical Detection

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

    PHELAN, JAMES M.

    2002-05-01

    Mine detection dogs have a demonstrated capability to locate hidden objects by trace chemical detection. Because of this capability, demining activities frequently employ mine detection dogs to locate individual buried landmines or for area reduction. The conditions appropriate for use of mine detection dogs are only beginning to emerge through diligent research that combines dog selection/training, the environmental conditions that impact landmine signature chemical vapors, and vapor sensing performance capability and reliability. This report seeks to address the fundamental soil-chemical interactions, driven by local weather history, that influence the availability of chemical for trace chemical detection. The processes evaluated include:more » landmine chemical emissions to the soil, chemical distribution in soils, chemical degradation in soils, and weather and chemical transport in soils. Simulation modeling is presented as a method to evaluate the complex interdependencies among these various processes and to establish conditions appropriate for trace chemical detection. Results from chemical analyses on soil samples obtained adjacent to landmines are presented and demonstrate the ultra-trace nature of these residues. Lastly, initial measurements of the vapor sensing performance of mine detection dogs demonstrates the extreme sensitivity of dogs in sensing landmine signature chemicals; however, reliability at these ultra-trace vapor concentrations still needs to be determined. Through this compilation, additional work is suggested that will fill in data gaps to improve the utility of trace chemical detection.« less

  8. Trace gas detection in hyperspectral imagery using the wavelet packet subspace

    NASA Astrophysics Data System (ADS)

    Salvador, Mark A. Z.

    This dissertation describes research into a new remote sensing method to detect trace gases in hyperspectral and ultra-spectral data. This new method is based on the wavelet packet transform. It attempts to improve both the computational tractability and the detection of trace gases in airborne and spaceborne spectral imagery. Atmospheric trace gas research supports various Earth science disciplines to include climatology, vulcanology, pollution monitoring, natural disasters, and intelligence and military applications. Hyperspectral and ultra-spectral data significantly increases the data glut of existing Earth science data sets. Spaceborne spectral data in particular significantly increases spectral resolution while performing daily global collections of the earth. Application of the wavelet packet transform to the spectral space of hyperspectral and ultra-spectral imagery data potentially improves remote sensing detection algorithms. It also facilities the parallelization of these methods for high performance computing. This research seeks two science goals, (1) developing a new spectral imagery detection algorithm, and (2) facilitating the parallelization of trace gas detection in spectral imagery data.

  9. Multivariate statistical analysis of the polyphenolic constituents in kiwifruit juices to trace fruit varieties and geographical origins.

    PubMed

    Guo, Jing; Yuan, Yahong; Dou, Pei; Yue, Tianli

    2017-10-01

    Fifty-one kiwifruit juice samples of seven kiwifruit varieties from five regions in China were analyzed to determine their polyphenols contents and to trace fruit varieties and geographical origins by multivariate statistical analysis. Twenty-one polyphenols belonging to four compound classes were determined by ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. (-)-Epicatechin, (+)-catechin, procyanidin B1 and caffeic acid derivatives were the predominant phenolic compounds in the juices. Principal component analysis (PCA) allowed a clear separation of the juices according to kiwifruit varieties. Stepwise linear discriminant analysis (SLDA) yielded satisfactory categorization of samples, provided 100% success rate according to kiwifruit varieties and 92.2% success rate according to geographical origins. The result showed that polyphenolic profiles of kiwifruit juices contain enough information to trace fruit varieties and geographical origins. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Trace and Ultra-trace Elements in the Deepest Part of the Vostok Ice Core, Antarctica: Geochemical Characterization of the Sub-glacial Lake Environment

    NASA Astrophysics Data System (ADS)

    Turetta, C.; Planchon, F.; Gabrielli, P.; Cozzi, G.; Cairns, W.; Barbaro, E.; Petit, J. R.; Bulat, S.; Boutron, C.; Barbante, C.

    2016-12-01

    We present in this study comprehensive data on the occurrence of 25 trace and ultra-trace elements in the deepest part of the Vostok ice core. The determination of Li, Na, Mg, Al, K, Ca, V, Cr, Mn, Fe, Co, Cu, Zn, As, Se, Rb, Sr, Mo, Ag, Cd, Sb, Ba, Pb, Bi and U has been performed in the different types of ice encountered from 3271 m to 3609 m of depth, corresponding to atmospheric ice, glacial flour and to accreted ice originating from the freezing of Lake Vostok waters. From atmospheric ice and glacial flour, the relative contributions of primary aerosols were evaluated for each element using a chemical mass balance approach in order to provide a first order evaluation of their partition between soluble (sea-salt) and insoluble (wind-blown dust) fractions in the ice. Sea-salt spray aerosols are the main source of impurities to the ice for certain elements (Na, Mg and K levels, and in a lesser extent to Ca, Sr, Rb, Li and U) while for other elements (Al, V, Cr, Mn, Fe, Co, Cu, Zn, Mo, Sb, Ba and Pb as well as the non sea salt fractions of Mg, K, Ca, Sr, Rb, Li and U) dust inputs appear to primarily control their depositional variability. For the glacial flour, the comparable levels of elements with the overlying atmospheric ice suggest that incorporation of abrasion debris at the glacier is quite limited in the sections considered. For the accreted ice originating from the subglacial waters of Lake Vostok, we observed a major chemical shift in the composition of the ice showing two distinct trends that we assumed to be derived from the chemical speciation of elements. The study of the glacier ice and the glacial flour has allowed us to perform a detailed characterisation of elemental abundances related to the aerosol sources variability and also to illustrate the interaction between the ice-sheet and the bedrock.

  11. Study of the Accumulation of Toxic and Essential Ultra-Trace Elements in Fruits of Sorbus domestica L.

    PubMed Central

    Zeiner, Michaela; Juranović Cindrić, Iva; Majić, Boris; Stingeder, Gerhard

    2017-01-01

    In the present work, the accumulation of selected toxic and essential ultra-trace elements in fruits of service tree (Sorbus domestica L.) were determined depending on harvest time. Samples were collected from the same sampling area in two different years and within one year in September and October (maturity state). Harvesting the fruits in the same area excludes the influence of metals taken up via roots, thus the impact of airborne contamination by heavy metal translocation can be studied. All samples were dried and digested using an acidic microwave assisted digestion system prior to quantification by inductively coupled plasma—sector field mass spectrometry (ICP–SFMS). The elements chosen were Arsenic and Cadmium as well as Lithium, Molybdenum, and Selenium. The Arsenic content rose with maturity in mesocarp. Cadmium found in the mesocarp was unaffected by ripeness. For Selenium and Molybdenum, no statistically significant effect of ripeness could be found on their content in mesocarp. Lithium could not be detected in the majority of fruit samples. Differences between the metal concentrations based on the year of harvest were found for Arsenic, Molybdenum, and Selenium, depending on precipitation. The drier the season, the more Arsenic was accumulated. For Molybdenum and Selenium, the opposite effect was observed. PMID:28338629

  12. Study of the Accumulation of Toxic and Essential Ultra-Trace Elements in Fruits of Sorbus domestica L.

    PubMed

    Zeiner, Michaela; Juranović Cindrić, Iva; Majić, Boris; Stingeder, Gerhard

    2017-03-24

    In the present work, the accumulation of selected toxic and essential ultra-trace elements in fruits of service tree ( Sorbus domestica L.) were determined depending on harvest time. Samples were collected from the same sampling area in two different years and within one year in September and October (maturity state). Harvesting the fruits in the same area excludes the influence of metals taken up via roots, thus the impact of airborne contamination by heavy metal translocation can be studied. All samples were dried and digested using an acidic microwave assisted digestion system prior to quantification by inductively coupled plasma-sector field mass spectrometry (ICP-SFMS). The elements chosen were Arsenic and Cadmium as well as Lithium, Molybdenum, and Selenium. The Arsenic content rose with maturity in mesocarp. Cadmium found in the mesocarp was unaffected by ripeness. For Selenium and Molybdenum, no statistically significant effect of ripeness could be found on their content in mesocarp. Lithium could not be detected in the majority of fruit samples. Differences between the metal concentrations based on the year of harvest were found for Arsenic, Molybdenum, and Selenium, depending on precipitation. The drier the season, the more Arsenic was accumulated. For Molybdenum and Selenium, the opposite effect was observed.

  13. Towards the interaction between calcium carbide and water during gas-chromatographic determination of trace moisture in ultra-high purity ammonia.

    PubMed

    Trubyanov, Maxim M; Mochalov, Georgy M; Suvorov, Sergey S; Puzanov, Egor S; Petukhov, Anton N; Vorotyntsev, Ilya V; Vorotyntsev, Vladimir M

    2018-07-27

    The current study focuses on the processes involved during the flow conversion of water into acetylene in a calcium carbide reaction cell for the trace moisture analysis of ammonia by reaction gas chromatography. The factors negatively affecting the reproducibility and the accuracy of the measurements are suggested and discussed. The intramolecular reaction of the HOCaCCH intermediate was found to be a side reaction producing background acetylene during the contact of wet ammonia gas with calcium carbide. The presence of the HOCaCCH intermediate among the reaction products is confirmed by an FTIR spectral study of calcium carbide powder exposed to wet gas. The side reaction kinetics is evaluated experimentally and its influence on the results of the gas chromatographic measurements is discussed in relation to the determination of the optimal operating parameters for ammonia analysis. The reaction gas chromatography method for the trace moisture measurements in an ammonia matrix was experimentally compared to an FTIR long-path length gas cell technique to evaluate the accuracy limitations and the resource intensity. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Ultra-rapid earth rotation determination with VLBI during CONT11 and CONT14

    NASA Astrophysics Data System (ADS)

    Haas, Rüdiger; Hobiger, Thomas; Kurihara, Shinobu; Hara, Tetsuya

    2015-08-01

    In 2007 the Geospatial Information Authority of Japan (GSI) and the Onsala Space Observatory (OSO) started a collaboration project aiming at determining the earth rotation angle, usually expressed as UT1-UTC, in near real-time. In the beginning of this project dedicated one hour long one-baseline experiments were observed periodically using the VLBI stations Onsala (Sweden) and Tsukuba (Japan). The strategy is that the observed VLBI data are sent in real-time via the international optical fibre backbone to the correlator at Tsukuba where the data are correlated with a software correlator and analyzed in near-real time with the c5++ VLBI data analysis software, thus producing UT1-UTC results with very low latency. The latency between the observation at the stations and the determination of UT1-UTC is on the order of a few minutes, thus we can talk about an ultra-rapid determination of UT1-UTC. An offline version of this strategy was adopted in 2009 for the regular VLBI intensive series INT-2, organized by the International VLBI Service for Geodesy and Astrometry (IVS), that involves Wettzell (Germany) and Tsukuba. Since March 2010 the INT-2 is using real-time e-transfer, too, and since June 2010 also automated analysis. Starting in 2009 the ultra-rapid approach was applied to regular 24 hour long IVS VLBI-sessions that involve Tsukuba and Onsala, so that ultra-rapid UT1-UTC results can be produced already during ongoing VLBI-sessions. This strategy was successfully operated during the 15 days long continuous VLBI campaigns CONT11 and CONT14. In this presentation we give an overview of the ultra-rapid concept, present the results derived during CONT11 and CONT14, and compare these ultra-rapid results to results derived from post-processing

  15. Ultra-rapid earth rotation determination with VLBI during CONT11 and CONT14

    NASA Astrophysics Data System (ADS)

    Haas, Rüdiger; Hobiger, Thomas; Kurihara, Shinobu; Hara, Tetsuya

    2016-04-01

    In 2007 the Geospatial Information Authority of Japan (GSI) and the Onsala Space Observatory (OSO) started a collaboration project aiming at determining the earth rotation angle, usually expressed as UT1-UTC, in near real-time. In the beginning of this project dedicated one hour long one-baseline experiments were observed periodically using the VLBI stations Onsala (Sweden) and Tsukuba (Japan). The strategy is that the observed VLBI data are sent in real-time via the international optical fibre backbone to the correlator at Tsukuba where the data are correlated with a software correlator and analyzed in near-real time with the c5++ VLBI data analysis software, thus producing UT1-UTC results with very low latency. The latency between the observation at the stations and the determination of UT1-UTC is on the order of a few minutes, thus we can talk about an ultra-rapid determination of UT1-UTC. An offline version of this strategy was adopted in 2009 for the regular VLBI intensive series INT-2, organized by the International VLBI Service for Geodesy and Astrometry (IVS), that involves Wettzell (Germany) and Tsukuba. Since March 2010 the INT-2 is using real-time e-transfer, too, and since June 2010 also automated analysis. Starting in 2009 the ultra-rapid approach was applied to regular 24 hour long IVS VLBI-sessions that involve Tsukuba and Onsala, so that ultra-rapid UT1-UTC results can be produced already during ongoing VLBI-sessions. This strategy was successfully operated during the 15 days long continuous VLBI campaigns CONT11 and CONT14. In this presentation we give an overview of the ultra-rapid concept, present the results derived during CONT11 and CONT14, and compare these ultra-rapid results to results derived from post-processing.

  16. Ultra-trace determination of Strontium-90 in environmental soil samples from Qatar by collision/reaction cell-inductively coupled plasma mass spectrometry (CRC-ICP-MS/MS)

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

    Al-Meer, S. H.; Amr, M. A.; Helal, A.I.

    Because of the very low level of {sup 90}Sr in the environmental soil samples and its determination by beta counting may take several weeks, we developed a procedure for ultra-trace determination of {sup 90}Sr using collision reaction cell-inductively coupled plasma tandem mass spectrometry (CRC-ICP-MS/MS, Agilent 8800). Soil samples were dried at 105 deg. C and then heated in a furnace at 550 deg. C to remove any organics present. 500 g of each soil samples were aliquoted into 2000 ml glass beakers. Each Soils samples were soaked in 2 ppm Sr solution carrier to allow determination of chemical yield. Themore » solid to liquid ratio was 1:1. Finally the soil samples were dried at 105 deg. C. Five hundred milliliters concentrated nitric acid and 250 ml hydrochloric acid volumes were added on 500 g soil samples. The samples were digested on hot plate at 80 deg. C to prevent spraying with continuous manual mixing. The leachate solution was separated. The solids were rinsed with 500 ml deionized water, warmed on a hot plate and the leachate plus previous leachate were filtered and the total volume was reduced to 500 ml by evaporation. Final leachate volume was transferred to a centrifuge tubes. The centrifuge tubes were centrifuged at 3,500 rpm for 10 min. The leachate was transferred to a 1 L beaker and heated on a hot plate to evaporate the leachate to dryness. The reside was re-dissolved in 100 ml of 2% HNO{sub 3} and reduced by evaporation to 10 mL. The solution was measured directly by CRC-ICP-MS/MS by setting the first quadruple analyzer to m/z 90 and introducing oxygen gas into the reaction cell for elimination isobar interference from zirconium-90. The method was validated by measurements of standard reference materials and applied on environmental soil samples. The overall time requirement for the measurement of strontium-90 by CRC-ICP-MS/MS is 2 days, significantly shorter than any radioanalytical protocol currently available. (authors)« less

  17. Determining thickness and refractive index from free-standing ultra-thin polymer films with spectroscopic ellipsometry

    DOE PAGES

    Hilfiker, James N.; Stadermann, Michael; Sun, Jianing; ...

    2016-08-27

    It is a well-known challenge to determine refractive index (n) from ultra-thin films where the thickness is less than about 10 nm. In this paper, we discovered an interesting exception to this issue while characterizing spectroscopic ellipsometry (SE) data from isotropic, free-standing polymer films. Ellipsometry analysis shows that both thickness and refractive index can be independently determined for free-standing films as thin as 5 nm. Simulations further confirm an orthogonal separation between thickness and index effects on the experimental SE data. Effects of angle of incidence and wavelength on the data and sensitivity are discussed. Finally, while others have demonstratedmore » methods to determine refractive index from ultra-thin films, our analysis provides the first results to demonstrate high-sensitivity to the refractive index from ultra-thin layers.« less

  18. In Situ Determination of Trace Elements in Fish Otoliths by Laser Ablation Double Focusing Sector Field Inductively Coupled Plasma Mass Spectrometry Using a Solution Standard Addition Calibration Method

    NASA Astrophysics Data System (ADS)

    Chen, Z.; Jones, C. M.

    2002-05-01

    Microchemistry of fish otoliths (fish ear bones) is a very useful tool for monitoring aquatic environments and fish migration. However, determination of the elemental composition in fish otolith by ICP-MS has been limited to either analysis of dissolved sample solution or measurement of limited number of trace elements by laser ablation (LA)- ICP-MS due to low sensitivity, lack of available calibration standards, and complexity of polyatomic molecular interference. In this study, a method was developed for in situ determination of trace elements in fish otoliths by laser ablation double focusing sector field ultra high sensitivity Finnigan Element 2 ICP-MS using a solution standard addition calibration method. Due to the lack of matrix-match solid calibration standards, sixteen trace elements (Na, Mg, P, Cr, Mn, Fe, Ni, Cu, Rb, Sr, Y, Cd, La, Ba, Pb and U) were determined using a solution standard calibration with Ca as an internal standard. Flexibility, easy preparation and stable signals are the advantages of using solution calibration standards. In order to resolve polyatomic molecular interferences, medium resolution (M/delta M > 4000) was used for some elements (Na, Mg, P, Cr, Mn, Fe, Ni, and Cu). Both external calibration and standard addition quantification strategies are compared and discussed. Precision, accuracy, and limits of detection are presented.

  19. Classroom Determination of Trace Organic Substances by Catalytic Methods.

    ERIC Educational Resources Information Center

    Wenck, Helmut; And Others

    1988-01-01

    Describes three trace determinations of organic substances utilizing a spectrophotometer. Provides procedures and absorbance wavelengths for determining acetonitrile, oxalic acid, and oxalic acid in human serum. Explores the role of acetonitrile and oxalic acid as catalysts in their respective reactions. (ML)

  20. Simultaneous determination of four water-soluble vitamins in fortified infant foods by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry.

    PubMed

    Lu, Baiyi; Ren, Yiping; Huang, Baifen; Liao, Wenqun; Cai, Zengxuan; Tie, Xiaowei

    2008-03-01

    A novel ultra-performance liquid chromatography electrospray ionization tandem triple quadrupole mass spectrometry method for the simultaneous determination of four water-soluble vitamins, including vitamin B5 (VB5), vitamin B8 (VB8), vitamin B9 (VB9), and vitamin B12 (VB12) in fortified infant foods is developed and validated. A reverse phase UPLC separation system consisting of a Waters ACQUITY UPLC BEH C-18 column (2.1 mm x 100 mm i.d., 1.7 microm) and a binary gradient acetonitrile-water mobile phase is applied for the separation of the four water-soluble vitamins. Formic acid is spiked into the mobile phase to enhance the ionization efficiency. Tandem MS-MS analysis is performed in multi-reaction monitoring mode (MRM). Product-ion traces at m/z 220.1 --> 89.9 for VB5, 245.1 --> 227.1 for VB8, 442.3 --> 295.2 for VB9, and 678.9 --> 147.0 for VB12 are used for quantitation of the corresponding vitamins, and traces at m/z 455.5 --> 308.0 are used for methotrexate (internal standard). Limits of quantitation (LOQs) are 0.016, 0.090, 0.020, and 0.019 microg/L for VB5, VB8, VB9, and VB12, respectively. Intra- and inter-day precisions for the determination of the four vitamins are better than 6.84% and 12.26% in relative standard deviations, and recoveries for the four vitamins are in the range of 86.0~101.5%. The developed approach is applied for the determination of the trace amounts of the vitamins in fortified milk powers and fortified rice powers.

  1. Ultra-sensitive Trace-Water Optical Sensor with In situ- synthesized Metal-Organic Framework in Glass Paper.

    PubMed

    Ohira, Shin-Ichi; Nakamura, Nao; Endo, Masaaki; Miki, Yusuke; Hirose, Yasuo; Toda, Kei

    2018-01-01

    Monitoring of trace water in industrial gases is strongly recommended because contaminants cause serious problems during use, especially in the semiconductor industry. An ultra-sensitive trace-water sensor was developed with an in situ-synthesized metal-organic framework as the sensing material. The sample gas is passed through the sensing membrane and efficiently and rapidly collected by the sensing material in the newly designed gas collection/detection cell. The sensing membrane, glass paper impregnated with copper 1,3,5-benzenetricarboxylate (Cu-BTC), is also newly developed. The amount and density of the sensing material in the sensing membrane must be well balanced to achieve rapid and sensitive responses. In the present study, Cu-BTC was synthesized in situ in glass paper. The developed system gave high sensing performances with a limit of detection (signal/noise ratio = 3) of 9 parts per billion by volume (ppbv) H 2 O and a 90% response time of 86 s for 200 ppbv H 2 O. The reproducibility of the responses within and between lots had relative standard deviations for 500 ppbv H 2 O of 0.8% (n = 10) and 1.5% (n = 3), respectively. The long-term (2 weeks) stability was 7.3% for 400 ppbv H 2 O and one-year continuous monitoring test showed the sensitivity change of <∼3% before and after the study. Furthermore, the system response was in good agreement with the response achieved in cavity ring-down spectroscopy. These performances are sufficient for monitoring trace water in industrial gases. The integrated system with light and gas transparent structure for gas collection/absorbance detection can also be used for other target gases, using specific metal-organic frameworks.

  2. Plutonium oxalate precipitation for trace elemental determination in plutonium materials

    DOE PAGES

    Xu, Ning; Gallimore, David; Lujan, Elmer; ...

    2015-05-26

    In this study, an analytical chemistry method has been developed that removes the plutonium (Pu) matrix from the dissolved Pu metal or oxide solution prior to the determination of trace impurities that are present in the metal or oxide. In this study, a Pu oxalate approach was employed to separate Pu from trace impurities. After Pu(III) was precipitated with oxalic acid and separated by centrifugation, trace elemental constituents in the supernatant were analyzed by inductively coupled plasma-optical emission spectroscopy with minimized spectral interferences from the sample matrix.

  3. Molecularly imprinted sensor based on Russian Matryoshka structured molecules for enhanced specific identification and double amplification in ultra-trace Tb3+ determination.

    PubMed

    Li, Jianping; Yang, Bin; Pan, Hongcheng; Xu, Guobao

    2018-06-30

    The selective and sensitive detection of rare earth elements is thought to be difficult because the concentration of those elements in the sample is commonly at a low level and they normally have severe mutual interference which is caused by homologous chemical properties. In this study, a novel molecularly imprinted polymer (MIP) sensor was fabricated for highly sensitive and selective determination of ultra-trace Tb 3+ . The Tb 3+ -ethylenediaminetetraacetic acid complex (Tb-EDTA) as the template molecule was incorporated into mono-6-mercapto-β-cyclodextrin (mono-6-SH-β-CD) to form a Russian Matryoshka (RM)-structured molecule (CD/Tb-EDTA). Titanium isopropoxide was utilized in vapor sol-gel polymerization to construct MIP membrane. Moreover, the selectivity of the RM MIP sensor was remarkably enhanced by the "triple-selectivity" recognition of EDTA-to-Tb 3+ , β-CD-to-(Tb-EDTA), and 3D cavity-to-(CD/Tb-EDTA), while the sensitivity of the MIP sensor was significantly improved by ECL signal enhancement based on double amplification, in other words, the electrochemiluminescence resonance energy transfer (ECL-RET) between the ECL donor of CD/Tb-EDTA and the ECL acceptor of Ru(bpy) 3 2+ , and the ECL enhancement by the co-reactant of CD/Tb-EDTA on Ru(bpy) 3 Cl 2 . When the imprinted cavities were occupied by Tb-EDTA during rebinding, the host-guest inclusion structured complex was formed and the ECL intensities produced by the Ru(bpy) 3 Cl 2 ECL system increased with increasing concentration of Tb-EDTA. The proposed sensor was used for quantitative analysis of Tb 3+ with concentrations ranging from 8.00 × 10 -13 mol/L to 4.00 × 10 -9 mol/L and successfully applied to detect Tb 3+ in seawater samples. The detection limit of the sensor was found to be 3.90 × 10 -13 mol/L (DL = 3δ b /K), which is lower than previously reported values. Thus, the fabricated sensor is feasible for practical applications. Copyright © 2018 Elsevier B.V. All rights

  4. The share of ultra-processed foods determines the overall nutritional quality of diets in Brazil.

    PubMed

    Louzada, Maria Laura da Costa; Ricardo, Camila Zancheta; Steele, Euridice Martinez; Levy, Renata Bertazzi; Cannon, Geoffrey; Monteiro, Carlos Augusto

    2018-01-01

    To estimate the dietary share of ultra-processed foods and to determine its association with the overall nutritional quality of diets in Brazil. Cross-sectional. Brazil. A representative sample of 32 898 Brazilians aged ≥10 years was studied. Food intake data were collected. We calculated the average dietary content of individual nutrients and compared them across quintiles of energy share of ultra-processed foods. Then we identified nutrient-based dietary patterns, and evaluated the association between quintiles of dietary share of ultra-processed foods and the patterns' scores. The mean per capita daily dietary energy intake was 7933 kJ (1896 kcal), with 58·1 % from unprocessed or minimally processed foods, 10·9 % from processed culinary ingredients, 10·6 % from processed foods and 20·4 % from ultra-processed foods. Consumption of ultra-processed foods was directly associated with high consumption of free sugars and total, saturated and trans fats, and with low consumption of protein, dietary fibre, and most of the assessed vitamins and minerals. Four nutrient-based dietary patterns were identified. 'Healthy pattern 1' carried more protein and micronutrients, and less free sugars. 'Healthy pattern 2' carried more vitamins. 'Healthy pattern 3' carried more dietary fibre and minerals and less free sugars. 'Unhealthy pattern' carried more total, saturated and trans fats, and less dietary fibre. The dietary share of ultra-processed foods was inversely associated with 'healthy pattern 1' (-0·16; 95 % CI -0·17, -0·15) and 'healthy pattern 3' (-0·18; 95 % CI -0·19, -0·17), and directly associated with 'unhealthy pattern' (0·17; 95 % CI 0·15, 0·18). Dietary share of ultra-processed foods determines the overall nutritional quality of diets in Brazil.

  5. Determination of Trace Concentration in TMD Detectors using PGAA

    NASA Astrophysics Data System (ADS)

    Tomandl, I.; Viererbl, L.; Kudějová, P.; Lahodová, Z.; Klupák, V.; Fikrle, M.

    2015-05-01

    Transmutation detectors could be alternative to the traditional activation detector method for neutron fluence dosimetry at power nuclear reactors. This new method require an isotopically highly-sensitive, non-destructive in sense of compactness as well as isotopic content, precise and standardly used analytical method for trace concentration determination. The capability of Prompt Gamma-ray Activation Analysis (PGAA) for determination of trace concentrations of transmuted stable nuclides in the metallic foils of Ni, Au, Cu and Nb, which were irradiated for 21 days in the reactor core at the LVR-15 research reactor in Řež, is reported. The PGAA measurements of these activation foils were performed at the PGAA facility at Forschungs-Neutronenquelle Heinz Maier-Leibnitz (FRMII) in Garching.

  6. [Determination and correlation analysis of trace elements in Boletus tomentipes].

    PubMed

    Li, Tao; Wang, Yuan-zhong; Zhang, Ji; Zhao, Yan-li; Liu, Hong-gao

    2011-07-01

    The contents of eleven trace elements in Boletus tomentipes were determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The results showed that the fruiting bodies of B. tomentipes were very rich in Mg and Fe (>100 mg x kg(-1)) and rich in Mn, Zn and Cu (>10 mg x kg(-1)). Cr, Pb, Ni, Cd, and As were relatively minor contents (0.1-10.0 mg x kg(-1)) of this species, while Hg occurred at the smallest content (< 0.1 mg x kg(-1)). Among the determined 11 trace elements, Zn-Cu had significantly positive correlation (r = 0.659, P < 0.05), whereas, Hg-As, Ni-Fe, and Zn-Mg had significantly negative correlation (r = -0.672, -0.610, -0.617, P < 0.05). This paper presented the trace elements properties of B. tomentipes, and is expected to be useful for exploitation and quality evaluation of this species.

  7. Determination of trace metals in drinking water in Irbid City-Northern Jordan.

    PubMed

    Alomary, Ahmed

    2013-02-01

    Drinking water samples from Irbid, the second populated city in Jordan were analyzed for trace metals (As, Ba, Cd, Pb, Cr, Cu, Fe, Zn, Mn, Ni, and Se) content. The study was undertaken to determine if the metal concentrations were within the national and international guidelines. A total of 90 drinking water samples were collected from Al-Yarmouk University area. The samples were collected from three different water types: tap water (TW), home-purified water (HPW), and plant-purified water (PPW). All the samples were analyzed for trace metals using an inductively coupled plasma-optical emission spectrometry. All the samples analyzed were within the United States Environmental Protection Agency admissible pH limit (6.5-8.5). The results showed that concentrations of the trace metals vary significantly between the three drinking water types. The results showed that HPW samples have the lowest level of trace metals and the concentrations of some essential trace metals in these samples are less than the recommended amounts. Slight differences in the metal contents were found between HPW samples, little differences between PPW samples; however, significant differences were found between TW samples. Although some TW samples showed high levels of trace metals, however, the mean level of most elements determined in the samples were well within the Jordanian standards as well as the World Health Organization standards for drinking water.

  8. Rapid ultra-trace analysis of sucralose in multiple-origin aqueous samples by online solid-phase extraction coupled to high-resolution mass spectrometry.

    PubMed

    Batchu, Sudha Rani; Ramirez, Cesar E; Gardinali, Piero R

    2015-05-01

    Because of its widespread consumption and its persistence during wastewater treatment, the artificial sweetener sucralose has gained considerable interest as a proxy to detect wastewater intrusion into usable water resources. The molecular resilience of this compound dictates that coastal and oceanic waters are the final recipient of this compound with unknown effects on ecosystems. Furthermore, no suitable methodologies have been reported for routine, ultra-trace detection of sucralose in seawater as the sensitivity of traditional liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis is limited by a low yield of product ions upon collision-induced dissociation (CID). In this work, we report the development and field test of an alternative analysis tool for sucralose in environmental waters, with enough sensitivity for the proper quantitation and confirmation of this analyte in seawater. The methodology is based on automated online solid-phase extraction (SPE) and high-resolving-power orbitrap MS detection. Operating in full scan (no CID), detection of the unique isotopic pattern (100:96:31 for [M-H](-), [M-H+2](-), and [M-H+4](-), respectively) was used for ultra-trace quantitation and analyte identification. The method offers fast analysis (14 min per run) and low sample consumption (10 mL per sample) with method detection and confirmation limits (MDLs and MCLs) of 1.4 and 5.7 ng/L in seawater, respectively. The methodology involves low operating costs due to virtually no sample preparation steps or consumables. As an application example, samples were collected from 17 oceanic and estuarine sites in Broward County, FL, with varying salinity (6-40 PSU). Samples included the ocean outfall of the Southern Regional Wastewater Treatment Plant (WWTP) that serves Hollywood, FL. Sucralose was detected above MCL in 78% of the samples at concentrations ranging from 8 to 148 ng/L, with the exception of the WWTP ocean outfall (at pipe end, 28 m below the surface

  9. [Determination of trace gallium by graphite furnace atomic absorption spectrometry in urine].

    PubMed

    Zhou, L Z; Fu, S; Gao, S Q; He, G W

    2016-06-20

    To establish a method for determination trace gallium in urine by graphite furnace atomic absorption spectrometry (GFAAS). The ammonium dihydrogen phosphate was matrix modifier. The temperature effect about pyrolysis (Tpyr) and atomization temperature were optimized for determination of trace gallium. The method of technical standard about within-run, between-run and recoveries of standard were optimized. The method showed a linear relationship within the range of 0.20~80.00 μg/L (r=0.998). The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 5.0, 10.0, 20.0 μg/L concentration levels were 2.1%~5.5% and 2.3%~3.0%. The detection limit was 0.06 μg/L. The recoveries of gallium were 98.2%~101.1%. This method is simple, low detection limit, accurate, reliable and reproducible. It has been applied for determination of trace gallium in urine samples those who need occupation health examination or poisoning diagnosis.

  10. Ultra high performance liquid chromatography tandem mass spectrometry for rapid analysis of trace organic contaminants in water

    PubMed Central

    2013-01-01

    Background The widespread utilization of organic compounds in modern society and their dispersion through wastewater have resulted in extensive contamination of source and drinking waters. The vast majority of these compounds are not regulated in wastewater outfalls or in drinking water while trace amounts of certain compounds can impact aquatic wildlife. Hence it is prudent to monitor these contaminants in water sources until sufficient toxicological data relevant to humans becomes available. A method was developed for the analysis of 36 trace organic contaminants (TOrCs) including pharmaceuticals, pesticides, steroid hormones (androgens, progestins, and glucocorticoids), personal care products and polyfluorinated compounds (PFCs) using a single solid phase extraction (SPE) technique with ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). The method was applied to a variety of water matrices to demonstrate method performance and reliability. Results UHPLC-MS/MS in both positive and negative electrospray ionization (ESI) modes was employed to achieve optimum sensitivity while reducing sample analysis time (<20 min) compared with previously published methods. The detection limits for most compounds was lower than 1.0 picogram on the column while reporting limits in water ranged from 0.1 to 15 ng/L based on the extraction of a 1 L sample and concentration to 1 mL. Recoveries in ultrapure water for most compounds were between 90-110%, while recoveries in surface water and wastewater were in the range of 39-121% and 38-141% respectively. The analytical method was successfully applied to analyze samples across several different water matrices including wastewater, groundwater, surface water and drinking water at different stages of the treatment. Among several compounds detected in wastewater, sucralose and TCPP showed the highest concentrations. Conclusion The proposed method is sensitive, rapid and robust; hence it can

  11. Trace determination of zinc by substoichiometric isotope dilution analysis

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

    Sandhya, D.; Priya, S.; Subramanian, M.O.S.

    1996-09-01

    A radiometric method based on substoichiometric isotope dilution analysis using 1,10-phenanthroline and a substoichiometric amount of eosin was developed for determining trace amounts of zinc. Evaluation of various metal ion interferences shows that as little as 0.2 {mu}g Zn could be determined in an aqueous-phase volume of 60 mL. The method has been successfully applied to the determination of Zn in city waste incineration ash, cadmium metal, Fourts-B tablets, Boro-plus ointment, and magnesium alloy samples. 12 refs., 3 figs., 3 tabs.

  12. Measurement of trace impurities in ultra pure hydrogen and deuterium at the parts-per-billion level using gas chromatography

    NASA Astrophysics Data System (ADS)

    Ganzha, V.; Ivshin, K.; Kammel, P.; Kravchenko, P.; Kravtsov, P.; Petitjean, C.; Trofimov, V.; Vasilyev, A.; Vorobyov, A.; Vznuzdaev, M.; Wauters, F.

    2018-02-01

    A series of muon experiments at the Paul Scherrer Institute in Switzerland deploy ultra-pure hydrogen active targets. A new gas impurity analysis technique was developed, based on conventional gas chromatography, with the capability to measure part-per-billion (ppb) traces of nitrogen and oxygen in hydrogen and deuterium. Key ingredients are a cryogenic admixture accumulation, a directly connected sampling system and a dedicated calibration setup. The dependence of the measured concentration on the sample volume was investigated, confirming that all impurities from the sample gas are collected in the accumulation column and measured with the gas chromatograph. The system was calibrated utilizing dynamic dilution of admixtures into the gas flow down to sub-ppb level concentrations. The total amount of impurities accumulated in the purification system during a three month long experimental run was measured and agreed well with the calculated amount based on the measured concentrations in the flow.

  13. Beat frequency quartz-enhanced photoacoustic spectroscopy for fast and calibration-free continuous trace-gas monitoring

    PubMed Central

    Wu, Hongpeng; Dong, Lei; Zheng, Huadan; Yu, Yajun; Ma, Weiguang; Zhang, Lei; Yin, Wangbao; Xiao, Liantuan; Jia, Suotang; Tittel, Frank K.

    2017-01-01

    Quartz-enhanced photoacoustic spectroscopy (QEPAS) is a sensitive gas detection technique which requires frequent calibration and has a long response time. Here we report beat frequency (BF) QEPAS that can be used for ultra-sensitive calibration-free trace-gas detection and fast spectral scan applications. The resonance frequency and Q-factor of the quartz tuning fork (QTF) as well as the trace-gas concentration can be obtained simultaneously by detecting the beat frequency signal generated when the transient response signal of the QTF is demodulated at its non-resonance frequency. Hence, BF-QEPAS avoids a calibration process and permits continuous monitoring of a targeted trace gas. Three semiconductor lasers were selected as the excitation source to verify the performance of the BF-QEPAS technique. The BF-QEPAS method is capable of measuring lower trace-gas concentration levels with shorter averaging times as compared to conventional PAS and QEPAS techniques and determines the electrical QTF parameters precisely. PMID:28561065

  14. [Determination of 11 industrial antioxidants in the aqueous simulants by ultra-performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Fan, Sai; Zou, Jianhong; Li, Liping; Zhang, Nan; Liu, Wei; Li, Bing; Zhao, Xudong; Wu, Guohua; Xue, Ying; Zhao, Rong

    2014-09-01

    An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed to identify and determine 11 industrial antioxidants in the aqueous simulants. A ProElut PLS SPE column was used for the enrichment, and an ACQUITY UPLC BEH C18 UPLC column (100 mm x 2.1 mm, 1.7 μm) was used for separation by the gradient elution with pure water and acetonitrile as the mobile phases. The MS/MS detection was performed with an electrospray ionization (ESI) source in negative mode. The external standard method was used for quantitation in the present study. The linear ranges of the 11 analytes were from 5.0 to 100 μg/L. The coefficients of correlation were greater than 0.995. The recoveries of blank aqueous simulants fortified with the 11 analytes at the levels of 5.0, 10.0 and 20.0 μg/L were 61.4% to 109.4% with the relative standard deviations varied from 3.9% to 18.2% (n = 6). The LODs and LOQs of the 11 analytes in aqueous simulants were 0.2-1.0 μg/L and 0.5-3.0 μg/L, respectively. This method is highly sensitive and accurate, and can be applied to the determination of the 11 trace industrial antioxidants in the aqueous simulants.

  15. Akaganeite decorated graphene oxide composite for arsenic adsorption/removal and its proconcentration at ultra-trace level.

    PubMed

    Chen, Ming-Li; Sun, Yan; Huo, Chun-Bao; Liu, Chen; Wang, Jian-Hua

    2015-07-01

    Carboxylic graphene oxide (GO-COOH) is decorated with akaganeite (β-FeOOH) to produce a β-FeOOH@GO-COOH nanocomposite. The nanocomposite acts as an efficient adsorption medium for the uptake of arsenite and arsenate within a wide range of pH 3-10, providing high adsorption capacities of 77.5mgg(-1) for As(III) and 45.7mgg(-1) for As(V), respectively. Adsorption efficiencies of 100% and 97% are achieved for 5 successive operation cycles for the removal of 100μgL(-1) As(V) and As(III) in 5 fresh portions of aqueous solution (1.0mL for each) with 3mg nanocomposite. After 20 successive adsorption cycles, removal efficiency of >80% is still maintained for both arsenate and arsenite. Further, a removal efficiency of >90% is obtained for 1000μgL(-1) As(V) with 3mg β-FeOOH@GO-COOH for 5 successive adsorption cycles, and the presence of 2000-fold SO4(2-), NO3(-), Cl(-) and Mg(2+) pose no interfering effect. β-FeOOH@GO-COOH also provides a promising medium for the preconcentration of ultra-trace inorganic arsenic. 1mg of nanocomposite is used to adsorb 0.1-3.00μgL(-1) As(V) in 4.0mL solution, and the retained arsenate is recovered by 400μL of NaOH (2molL(-1), containing 2.0% NaBH4), followed by detection with atomic fluorescence spectrometry. A detection limit of 29ngL(-1) is obtained for arsenate. This procedure is validated by analyzing arsenic in a certified reference material (GBW 09101b) and further applied for arsenic determination in water samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. A simple, rapid and novel method based on salting-out assisted liquid-liquid extraction for ochratoxin A determination in beer samples prior to ultra-high performance liquid chromatography coupled to tandem mass spectrometry.

    PubMed

    Mariño-Repizo, Leonardo; Goicoechea, Hector; Raba, Julio; Cerutti, Soledad

    2018-06-07

    A novel, simple, easy and cheap sample treatment strategy based on salting-out assisted liquid-liquid extraction (SALLE) for ochratoxin A (OTA) ultra-trace analysis in beer samples using ultra-high performance liquid chromatography-tandem mass spectrometry determination was developed. The factors involved in the efficiency of pretreatment were studied employing factorial design in the screening phase and the optimal conditions of the significant variables on the analytical response were evaluated using a central composite face-centred design (CCF). Consequently, the amount of salt ((NH 4 ) 2 SO 4 ), together with the volumes of sample, hydrophilic (acetone) and nonpolar (toluene) solvents, and times of vortexing and centrifugation were optimized. Under optimized conditions, the limits of detection (LOD) and quantification (LOQ) were 0.02 µg l -1 and 0.08 µg l -1 respectively. OTA extraction recovery by SALLE was approximately 90% (0.2 µg l -1 ). Furthermore, the methodology was in agreement with EU Directive requirements and was successfully applied for analysis of beer samples.

  17. Quantitative Determining of Ultra-Trace Aluminum Ion in Environmental Samples by Liquid Phase Microextraction Assisted Anodic Stripping Voltammetry.

    PubMed

    Zhang, Liuyang; Luo, Jinju; Shen, Xinyu; Li, Chunya; Wang, Xian; Nie, Bei; Fang, Huaifang

    2018-05-10

    Direct detecting of trace amount Al(III) in aqueous solution by stripping voltammetry is often frustrated by its irreversible reduction, resided at −1.75 V (vs. Ag/AgCl reference), which is in a proximal potential of proton reduction. Here, we described an electroanalytical approach, combined with liquid phase microextraction (LPME) using ionic liquid (IL), to quantitatively assess trace amount aluminum in environmental samples. The Al(III) was caged by 8-hydroxyquinoline, forming a superb hydrophobic metal⁻chelate, which sequentially transfers and concentrates in the bottom layer of IL-phase during LPME. The preconcentrated Al(III) was further analyzed by a square-wave anodic stripping voltammetry (SW-ASV). The resulting Al-deposited electrodes were characterized by scanning electron microscopy and powder X-ray diffraction, showing the intriguing amorphous nanostructures. The method developed provides a linear calibration ranging from 0.1 to 1.2 ng L −1 with a correlation coefficient of 0.9978. The LOD attains as low as 1 pmol L −1 , which reaches the lowest report for Al(III) detection using electroanalytical techniques. The applicable methodology was implemented for monitoring Al(III) in commercial distilled water.

  18. Trace Determination of Linear Alkylbenzene Sulfonates: Application in Artificially Polluted Soil—Carrots System

    PubMed Central

    Sablayrolles, Caroline; Montréjaud-Vignoles, Mireille; Silvestre, Jérôme; Treilhou, Michel

    2009-01-01

    Surfactants are widely used in household and industrial products. The risk of incorporation of linear alkylbenzene sulfonates (LAS) from biosolids, wastewater, and fertilizers land application to the food chain is being assessed at present by the European Union. In the present work, a complete analytical method for LAS trace determination has been developed and successfully applied to LAS (C10–C13) uptake in carrot plants used as model. These carrots were grown in soil with the trace organics compounds added directly into the plant containers in pure substances form. LAS trace determination (μg kg−1 dry matter) in carrots samples was achieved by Soxtec apparatus and high-performance liquid chromatography-fluorescence detection. The methodology developed provides LAS determination at low detection limits (5 μg kg−1 dry matter) for carrot sample (2 g dry matter) with good recoveries rate (>90%). Transfer of LAS has been followed into the various parts of the carrot plant. LAS are generally found in the carrot leaves and percentage transfer remains very low (0.02%). PMID:20107562

  19. Kinetic determinations of trace element bioaccumulation in the mussel Mytilus edulis

    USGS Publications Warehouse

    Wang, W.-X.; Fisher, N.S.; Luoma, S.N.

    1996-01-01

    Laboratory experiments employing radiotracer methodology were conducted to determine the assimilation efficiencies from ingested natural seston, the influx rates from the dissolved phase and the efflux rates of 6 trace elements (Ag, Am, Cd, Co, Se and Zn) in the mussel Mytilus edulis. A kinetic model was then employed to predict trace element concentration in mussel tissues in 2 locations for which mussel and environmental data are well described: South San Francisco Bay (California, USA) and Long Island Sound (New York, USA). Assimilation efficiencies from natural seston ranged from 5 to 18% for Ag, 0.6 to 1% for Am, 8 to 20% for Cd, 12 to 16% for Co, 28 to 34% for Se, and 32 to 41% for Zn. Differences in chlorophyll a concentration in ingested natural seston did not have significant impact on the assimilation of Am, Co, Se and Zn. The influx rate of elements from the dissolved phase increased with the dissolved concentration, conforming to Freundlich adsorption isotherms. The calculated dissolved uptake rate constant was greatest for Ag, followed by Zn > Am = Cd > Co > Se. The estimated absorption efficiency from the dissolved phase was 1.53% for Ag, 0.34% for Am, 0.31% for Cd, 0.11% for Co, 0.03% for Se and 0.89% for Zn. Salinity had an inverse effect on the influx rate from the dissolved phase and dissolved organic carbon concentration had no significant effect on trace element uptake. The calculated efflux rate constants for all elements ranged from 1.0 to 3.0% d-1. The route of trace element uptake (food vs dissolved) and the duration of exposure to dissolved trace elements (12 h vs 6 d) did not significantly influence trace element efflux rates. A model which used the experimentally determined influx and efflux rates for each of the trace elements, following exposure from ingested food and from water, predicted concentrations of Ag, Cd, Se and Zn in mussels that were directly comparable to actual tissue concentrations independently measured in the 2

  20. [Determination of Trace Elements in Marine Cetaceans by ICP-MS and Health Risk Assessment].

    PubMed

    Ding, Yu-long; Ning, Xi; Gui, Duan; Mo, Hui; Li, Yu-sen; Wu, Yu-ping

    2015-09-01

    The liver, kidney and muscle samples from seven cetaceans were digested by microwave digestion, and trace elements amounts of V, Cd, Cu, Zn, As, Cr, Ni, Mn, Se, Hg and Pb were determined by inductively coupled plasma mass spectrometry (ICP-MS), and the health risk assessment for Zn, Cu, Cd, Hg, Se in the liver was conducted. The results of international lobster hepatopancreas standard (TORT-2) showed acceptable agreement with the certified values, and the relative standard deviation (RSD) of eleven kinds of trace elements were less than 3.54%, showing that the method is suitable for the determination of trace elements in cetaceans. The experimental results indicated that different tissues and organs of the dolphins had different trace elements, presenting the tissue specificity. There is a certain inter-species difference among different dolphins about the bioaccumulation ability of the trace elements. The distribution of trace elements in whales presented a certain regularity: the contents of most elements in liver, kidney were much higher than the contents of muscle tissues, Cu, Mn, Hg, Se, and Zn exhibit the higher concentrations in liver, while Cd was mainly accumulated in kidney. And according to the health risk assessment in liver, the exceeding standardrate of selenium and copper in seven kinds of whales was 100%, suggesting that these whales were suffering the contamination of trace elements. The experimental results is instructive to the study of trace elements in cetaceans, while this is the first report for the concentrations in organs of Striped dolphin, Bottlenose dolphin, Fraser's Dolphin and Risso's dolphin in China, it may provide us valuable data for the conservation of cetaceans.

  1. Multielement extraction system for the determination of 18 trace elements in geochemical samples

    USGS Publications Warehouse

    Clark, J.R.; Viets, J.G.

    1981-01-01

    A Methyl isobutyl ketone-Amine synerGistic Iodide Complex (MAGIC) extraction system has been developed for use in geochemical exploration which separates a maximum number of trace elements from interfering matrices. Extraction curves for 18 of these trace elements are presented: Pd, Pt, Cu, Ag, Au, Zn, Cd, Hg, Ga, In, Tl, Sa, Pb, As, Sb, Bi, Se, and Te. The acid normality of the aqueous phase controls the extraction into the organic phase, and each of these 18 elements has a broad range of HCl normality over which H is quantitatively extracted, making H possible to determine all 18 trace elements from a single sample digestion or leach solution. The extract can be analyzed directly by flame atomic absorption or inductively coupled plasma emission spectroscopy. Most of these 18 elements can be determined by Nameless atomic absorption after special treatment of the organic extract.

  2. Geochemical and isotopic determination of deep groundwater contributions and salinity to the shallow groundwater and surface water systems, Mesilla Basin, New Mexico, Texas, and Mexico

    NASA Astrophysics Data System (ADS)

    Robertson, A.; Carroll, K. C.; Kubicki, C.; Purtshert, R.

    2017-12-01

    The Mesilla Basin/Conejos-Médanos aquifer system, extending from southern New Mexico to Chihuahua, Mexico, is a priority transboundary aquifer under the 2006 United States­-Mexico Transboundary Aquifer Assessment Act. Declining water levels, deteriorating water quality, and increasing groundwater use by municipal, industrial, and agricultural users on both sides of the international border raise concerns about long-term aquifer sustainability. Relative contributions of present-day and "paleo" recharge to sustainable fresh groundwater yields has not been determined and evidence suggests that a large source of salinity at the distal end of the Mesilla Basin is saline discharge from deep groundwater flow. The magnitude and distribution of those deep saline flow paths are not determined. The contribution of deep groundwater to discharge and salinity in the shallow groundwater and surface water of the Mesilla Basin will be determined by collecting discrete groundwater samples and analyzing for aqueous geochemical and isotopic tracers, as well as the radioisotopes of argon and krypton. Analytes include major ions, trace elements, the stable isotopes of water, strontium and boron isotopes, uranium isotopes, the carbon isotopes of dissolved inorganic carbon, noble gas concentrations and helium isotope ratios. Dissolved gases are extracted and captured from groundwater wells using membrane contactors in a process known as ultra-trace sampling. Gas samples are analyzed for radioisotope ratios of krypton by the ATTA method and argon by low-level counting. Effectiveness of the ultra-trace sampling device and method was evaluated by comparing results of tritium concentrations to the krypton-85 content. Good agreement between the analyses, especially in samples with undetectable tritium, indicates that the ultra-trace procedure is effective and confirms that introduction of atmospheric air has not occurred. The geochemistry data indicate a complex system of geochemical

  3. Same-sample determination of ultratrace levels of polybromodiphenylethers, polybromodibenzo-p-dioxins/furans, and polychlorodibenzo-p-dioxins/furans from combustion flue gas

    EPA Science Inventory

    The analytical method used for determination of polychlorinated dibenzo-p-dioxins and -furans (PCDDs/Fs) emissions from municipal waste combustors and other stationary sources was modified and validated to enable simultaneous analysis of ultra trace levels of polybrominated diphe...

  4. Latest developments for low-power infrared laser-based trace gas sensors for sensor networks

    NASA Astrophysics Data System (ADS)

    So, Stephen; Thomazy, David; Wang, Wen; Marchat, Oscar; Wysocki, Gerard

    2011-09-01

    Academic and industrial researchers require ultra-low power, compact laser based trace-gas sensor systems for the most demanding environmental and space-borne applications. Here the latest results from research projects addressing these applications will be discussed: 1) an ultra-compact CO2 sensor based on a continuous wave quantum cascade laser, 2) an ultra-sensitive Faraday rotation spectrometer for O2 detection, 3) a fully ruggedized compact and low-power laser spectrometer, and 4) a novel non-paraxial nonthin multipass cell. Preliminary tests and projection for performance of future sensors based on this technology is presented.

  5. Determination of trace arsenic on hanging copper amalgam drop electrode.

    PubMed

    Piech, Robert; Baś, Bogusław; Niewiara, Ewa; Kubiak, Władysław W

    2007-04-30

    Hanging copper amalgam drop electrode has been applied for trace determination of arsenic by cathodic stripping analysis. Detection limit for As(III) as low as 0.33nM (0.02mug/L) at deposition time (240s) could be obtained. For seven successive determinations of As(III) at concentration of 5nM relative standard deviation was 2.5% (n=7). Interferences from selected metals and surfactant substances were examined. Absence of copper ions in sample solution causes easier optimization and makes method less vulnerable on contamination. The developed method was validated by analysis of certified reference materials (CRMs) and applied to arsenic determinations in natural water samples.

  6. A SIMS study of lunar 'komatiitic glasses' - Trace element characteristics and possible origin

    NASA Technical Reports Server (NTRS)

    Shearer, C. K.; Papike, J. J.; Galbreath, K. C.; Wentworth, S. J.; Shimizu, N.

    1990-01-01

    In Apollo 16 regolith breccias, Wentworth and McKay (1988) identified a suite of minute (less than 120 microns) 'komatiitic glass beads'. The wide major element compositional range, and ultra-Mg-prime character of the glasses suggest a variety of possible origins from complex impact processes to complex volcanic processes involving rather unusual and primitive magmatism. The extent of trace element depletion or enrichment in these glasses appears to be correlated to the siderophile character of the element (ionization potential or experimentally determined silicate melt/Fe metal partition coefficients. The ultra-Mg-prime glasses are depleted in Co relative to a bulk Moon Mg/Co exhibited by many lunar samples (volcanic glasses, basalts, regolith breccia, estimated upper mantle). The low Co and high incompatible element concentrations diminish the possibility that these glasses are a product of lunar komatiitic volcanism or impact, excavation, and melting of a very high Mg-prime plutonic unit.

  7. Determination of trace amount of formaldehyde base on a bromate-Malachite Green system.

    PubMed

    Tang, Yufang; Chen, Hao; Weng, Chao; Tang, Xiaohui; Zhang, Miaoling; Hu, Tao

    2015-01-25

    A novel catalytic kinetic spectrophotometric method for determination of trace amount of formaldehyde (FA) has been established, based on catalytic effect of trace amount of FA on the oxidation of Malachite Green (MG) by potassium bromate in presence of sulfuric acid medium, and was reported for the first time. The method was monitored by measuring the decrease in absorbance of MG at 617 nm and allowed a precise determination of FA in the range of 0.003-0.08 μg mL(-1), with a limit of detection down to 1 ng mL(-1). The relative standard deviation of 10 replicate measurements was 1.63%. The method developed was approved to be sensitive, selective and accurate, and adopted to determinate free FA in samples directly with good accuracy and reproducibility. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. A simple {sup 197}Hg RNAA procedure for the determination of mercury in urine, blood, and tissue

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

    Blotcky, A.J.; Rack, E.P.; Meade, A.G.

    1995-12-31

    Mercury has been implicated as a causal agent in such central nervous system diseases as Alzheimer`s and Parkinson`s. Consequently, there has been increased interest in the determination of ultra-trace-level mercury in biological matrices, especially in tissue. While such nonnuclear techniques as cold vapor atomic absorption spectrometry and cold vapor atomic fluorescence spectrometry have been employed routinely for mercury determinations in urine and blood, there is a paucity of nonnuclear techniques for the determination of mercury in the low parts-per-billion range in biological tissue. As pointed out by Fardy and Warner, instrumental and radiochemical neutron activation analysis (INAA and RNAA) requiremore » no blank determinations in contrast to nonnuclear analytical techniques employing digestion and/or chemical operations. Therefore, INAA and RNAA become the obvious choices for determination of ultra-trace levels of mercury in tissue. Most separation methods reported in the literature require different and separate methodologies for mercury determinations in urine, blood, or tissue. The purposes of this study are to develop a single methodology for the determination of low levels of mercury in all biological matrices by RNAA and to optimize parameters necessary for an efficacious trace-level determination. Previously, few studies have taken into account the effects of the Szilard-Chalmers reactions of the radioactivatable analyte within a biological matrix. It also would appear that little attention has been given to the optimum postirradiation carrier concentration of the analyte species necessary. This study discusses these various considerations.« less

  9. Determination of trace and heavy metals in some commonly used medicinal herbs in Ayurveda.

    PubMed

    Nema, Neelesh K; Maity, Niladri; Sarkar, Birendra K; Mukherjee, Pulok K

    2014-11-01

    Traditionally, the herbal drugs are well established for their therapeutic benefits. Depending upon their geographical sources sometimes the trace and heavy metals' content may differ, which may lead to severe toxicity. So, the toxicological and safety assessment of these herbal drugs are one of the major issues in recent days. Eight different plant species including Aloe vera, Centella asiatica, Calendula officinalis, Cucumis sativus, Camellia sinensis, Clitoria ternatea, Piper betel and Tagetes erecta were selected to determine their heavy and trace metals content and thereby to assure their safer therapeutic application. The trace and heavy metals were detected through atomic absorption spectrometry analysis. The selected medicinal plant materials were collected from the local cultivated regions of West Bengal, India, and were digested with nitric acid and hydrochloric acid as specified. Absorbance was measured through atomic absorption spectrometer (AA 303) and the concentration of different trace and heavy metals in the plant samples were calculated. The quantitative determinations were carried out using standard calibration curve obtained by the standard solutions of different metals. The contents of heavy metals were found to be within the prescribed limit. Other trace metals were found to be present in significant amount. Thus, on the basis of experimental outcome, it can be concluded that the plant materials collected from the specific region are safe and may not produce any harmful effect of metal toxicity during their therapeutic application. The investigated medicinal plants contain trace metals such as copper (Cu), chromium (Cr), manganese (Mn), iron (Fe) and nickel (Ni) as well as heavy metals such as arsenic (As), lead (Pb) and mercury (Hg), which were present within the permissible limit. © The Author(s) 2012.

  10. Determination of trace elements in dairy milk collected from the environment of coal-fired power plant.

    PubMed

    Ramamurthy, N; Thillaivelavan, K

    2005-01-01

    In the present study the environmental effects on herbivores mammals in and around Coal-fired power plant were studied by collecting the various milk samples of Cow and Buffalo in clean polyethylene bottles. Milk samples collected at five different locations along the banks of the Paravanaru river in and around Neyveli area. These samples were prepared for trace metal determination. The concentration of trace metals (Cu, Zn, Ni, Cd, Cr, Mn, Co and Hg) were determined by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Cold Vapour Atomic Absorption Spectrometry (CVAAS). It is observed that the samples contain greater amounts of trace metals than that in the unexposed areas. Obviously the milk samples are contaminated with these metals due to fly ash released in such environment.

  11. Determination of bisphenol AF (BPAF) in tissues, serum, urine and feces of orally dosed rats by ultra-high-pressure liquid chromatography-electrospray tandem mass spectrometry.

    PubMed

    Yang, Yunjia; Yin, Jie; Yang, Yi; Zhou, Naiyuan; Zhang, Jing; Shao, Bing; Wu, Yongning

    2012-07-15

    As a homologue of bisphenol A (BPA), there is concern about the potential reproductive and developmental toxicity of bisphenol AF (BPAF) based on in vitro tests. In this study, a simple and universal analytical method was developed for the determination of trace BPAF in various tissues and excreta of rats after they were orally dosed. The samples were hydrolyzed with glucuronidase/arylsulfatase followed by ultrasonic extraction with acetonitrile. The crude extract was purified with a mixed-mode anion exchange (Oasis MAX) solid-phase extraction (SPE) cartridge. Separation and quantification was then conducted by ultra-high-pressure liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in negative ionization mode. The recoveries at three fortification levels in different biological samples were from 71.0% to 102.3% with relative standard deviations no more than 13.2% (n=6). The quantification limits of the method were from 0.5 μg/kg to 3 μg/kg depending on the matrix. This method was successfully applied to the determination of BPAF in tissues, serum, urine and feces of orally dosed rats. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. The measurement of trace elements in interplanetary dust and cometary particles by ultra-high sensitivity INAA

    NASA Technical Reports Server (NTRS)

    Zolensky, M. E.; Lindstrom, David J.; Lindstrom, Richard M.; Lindstrom, M. M.

    1989-01-01

    Today the major elemental composition of interplanetary dust particles (IDPs) is routinely determined in many laboratories. These and mineralogical studies have revealed the presence of at least two major types of IDPs, chondritic and refractory. Preliminary results of a successful attempt to determine abundances of a large suite of trace elements from both chondritic and refractory IDPs are reported. The analytical procedure can be used in the grain-by-grain analysis of returned cometary samples. Chondritic and refractory IDPs are characterized by standard scanning electron microscopy and energy dispersive x ray spectroscopy (SEM-EDX) techniques. With this system, detection limits for many elements are well below picogram levels, and some approach femtogram levels. This technique is non-destructive, although some sample handling is required, so particles can be analyzed by other techniques after instrument neutron activation analysis (INAA) is completed. Data is presently being reduced from the analyses of 7 IDPs. These are U2015E10, U2015F1, W7029-A2, W7029-A3, W7013A8, LACl (all chondritic) and 705 (refractory). So far, 17 different major and trace elements were detected and measured in these particles, including rare earths and some very volatile elements (Br and Zn).

  13. [Determination of trace heavy metal elements in cortex Phellodendron chinense by ICP-MS after microwave-assisted digestion].

    PubMed

    Kou, Xing-Ming; Xu, Min; Gu, Yong-Zuo

    2007-06-01

    An inductively coupled plasma mass spectrometry (ICP-MS) for determination of the contents of 8 trace heavy metal elements in cortex Phellodendron chinense after microwave-assisted digestion of the sample has been developed. The accuracy of the method was evaluated by the analysis of corresponding trace heavy metal elements in standard reference materials (GBW 07604 and GBW 07605). By applying the proposed method, the contents of 8 trace heavy metal elements in cortex Phellodendron chinense cultivated in different areas (in Bazhong, Yibin and Yingjing, respectively) of Sichuan and different growth period (6, 8 and 10 years of samples from Yingjing) were determined. The relative standard deviation (RSD) is in the range of 3.2%-17.8% and the recoveries of standard addition are in the range of 70%-120%. The results of the study indicate that the proposed method has the advantages of simplicity, speediness and sensitivity. It is suitable for the determination of the contents of 8 trace heavy metal elements in cortex Phellodendron chinense. The results also show that the concentrations of 4 harmful trace heavy metal elements As, Cd, Hg and Pb in cortex Phellodendron chinense are all lower than the limits of Chinese Pharmacopoeia and Green Trade Standard for Importing and Exporting Medicinal Plant and Preparation. Therefore, the cortex Phellodendron chinense is fit for use as medicine and export.

  14. Ultra-high-pressure liquid chromatography-tandem mass spectrometry method for the determination of alkylphenols in soil.

    PubMed

    Wang, Jing; Pan, Hefang; Liu, Zhengzheng; Ge, Fei

    2009-03-20

    A novel method has been developed for the determination of alkylphenols in soil by ultra-high-pressure liquid chromatography employing small particle sizes, combined with tandem mass spectrometry. Soil samples were extracted with pressurized liquid extraction (PLE) and then cleaned with solid-phase extraction (SPE). The extracts were separated on C18 column (1.7 microm, 50 mm x 2.1mm) with a gradient elution and a mobile phase consisting of water and acetonitrile, and then detected by an electrospray ionization tandem mass spectrometry in negative ion mode with multiple reaction monitoring (MRM). Compared with traditional liquid chromatography, it took ultra-high-pressure liquid chromatography much less time to analyze alkylphenols. Additionally, the ultra-high-pressure liquid chromatography/tandem mass spectrometry method produces satisfactory reliability, sensitivity, and accuracy. The average recoveries of the three target analytes were 74.0-103.4%, with the RSD<15%. The calibration curves for alkylphenols were linear within the range of 0.01-0.4 microg/ml, with the correlation coefficients greater than 0.99. When 10 g soil sample was used for analysis, the limits of quantification (LOQs) of the three alkylphenols were all 1.0 microg/kg.

  15. Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

    PubMed

    Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

    2016-02-01

    A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

  16. Determination of Pb in Biological Samples by Graphite Furnace Atomic Absorption Spectrophotometry: An Exercise in Common Interferences and Fundamental Practices in Trace Element Determination

    ERIC Educational Resources Information Center

    Spudich, Thomas M.; Herrmann, Jennifer K.; Fietkau, Ronald; Edwards, Grant A.

    2004-01-01

    An experiment is conducted to ascertain trace-level Pb in samples of bovine liver or muscle by applying graphite furnace atomic absorption spectrophotometry (GFAAS). The primary objective is to display the effects of physical and spectral intrusions in determining trace elements, and project the usual methods employed to minimize accuracy errors…

  17. Determination of Serum Trace Elements (Zn, Cu, and Fe) in Pakistani Patients with Rheumatoid Arthritis.

    PubMed

    Ullah, Zia; Ullah, Muhammad Ikram; Hussain, Shabbir; Kaul, Haiba; Lone, Khalid P

    2017-01-01

    Rheumatoid arthritis (RA) is a chronic autoimmune inflammatory disease, which mainly involves the joints. RA is prevalent worldwide with increasing prevalence in elderly people. The mechanism of RA pathogenesis is still undefined, and it is interplaying between genetic susceptibility and environmental factors. Although risk factors for RA are not fully established, various studies have focused on the role of trace elements in association with RA. Trace elements act as co-factors for most of the enzymes, and their deficiency is associated with many untoward effects on human health. The homeostatic alterations in the metabolism of trace elements may partly be due to inflammatory response in RA. The objective of the present study was to determine the serum concentrations and correlation of zinc, copper, and iron in RA patients and healthy controls. The study comprised of 61 RA patients and 61 age- and sex-related healthy individuals of Pakistani population. Serum levels of Zn, Cu, and Fe were measured in all the participants by atomic absorption spectrophotometer. Serum Zn and Fe were significantly reduced in the RA patients than those in the healthy controls. Serum Cu concentrations were found elevated in the RA patients. Correlation studies of trace elements determine that there was negative correlation between Zn and Cu in the RA patients and no correlation in the control group. It is very important to explore the deficiency of essential trace metals in biological samples of the RA patients in different populations which may be helpful for diagnosis and supplementary management of rheumatoid arthritis patients.

  18. Quantitative Ultrasound-Assisted Extraction for Trace-Metal Determination: An Experiment for Analytical Chemistry

    ERIC Educational Resources Information Center

    Lavilla, Isela; Costas, Marta; Pena-Pereira, Francisco; Gil, Sandra; Bendicho, Carlos

    2011-01-01

    Ultrasound-assisted extraction (UAE) is introduced to upper-level analytical chemistry students as a simple strategy focused on sample preparation for trace-metal determination in biological tissues. Nickel extraction in seafood samples and quantification by electrothermal atomic absorption spectrometry (ETAAS) are carried out by a team of four…

  19. Determination of trace elements and their concentrations in clay balls: problem of geophagia practice in Ghana.

    PubMed

    Arhin, Emmanuel; Zango, Musah S

    2017-02-01

    Ten samples of 100 g weight were subsampled from 1400 g of the clay balls from which the contained trace element levels were determined by X-ray fluorescence technique. The results of trace elements in the clay balls were calibrated using certified reference materials "MAJMON" and "BH-1." The results showed elevated concentrations but with different concentration levels in the regions, particularly with arsenic, chromium, cobalt, Cs, Zr and La. These trace elements contained in the clay balls are known to be hazardous to human health. Thence the relatively high concentrations of these listed trace elements in clay balls in the three regions, namely Ashanti, Upper East and Volta, which are widely sold in markets in Ghana, could present negative health impact on consumers if consumed at 70 g per day or more and on regular basis. On the basis of these, the study concludes an investigation to establish breakeven range for trace element concentrations in the clay balls as it has been able to demonstrate the uneven and elevated values in them. The standardized safe ranges of trace elements will make the practice safer for the people that ingest clay balls in Ghana.

  20. Analysis of ultra-triathlon performances

    PubMed Central

    Lepers, Romuald; Knechtle, Beat; Knechtle, Patrizia; Rosemann, Thomas

    2011-01-01

    Despite increased interest in ultra-endurance events, little research has examined ultra-triathlon performance. The aims of this study were: (i) to compare swimming, cycling, running, and overall performances in three ultra-distance triathlons, double Ironman distance triathlon (2IMT) (7.6 km swimming, 360 km cycling, and 84.4 km running), triple Ironman distance triathlon (3IMT) (11.4 km, 540 km, and 126.6 km), and deca Ironman distance triathlon (10IMT) (38 km, 1800 km, and 420 km) and (ii) to examine the relationships between the 2IMT, 3IMT, and 10IMT performances to create predicted equations of the 10IMT performances. Race results from 1985 through 2009 were examined to identify triathletes who performed the three considered ultra-distances. In total, 73 triathletes (68 men and 5 women) were identified. The contribution of swimming to overall ultra-triathlon performance was lower than for cycling and running. Running performance was more important to overall performance for 2IMT and 3IMT compared with 10IMT The 2IMT and 3IMT performances were significantly correlated with 10IMT performances for swimming and cycling, but not for running. 10IMT total time performance might be predicted by the following equation: 10IMT race time (minutes) = 5885 + 3.69 × 3IMT race time (minutes). This analysis of human performance during ultra-distance triathlons represents a unique data set in the field of ultra-endurance events. Additional studies are required to determine the physiological and psychological factors associated with ultra-triathlon performance. PMID:24198579

  1. Determination of trace elements in Ethiopian, Vietnamese, and Japanese women using high-resolution IC-PMS.

    PubMed

    Tekeste, Zinaye; Amare, Bemnet; Asfaw, Fanaye; Fantahun, Bereket; van Nguyen, Nhien; Nishikawa, Takeshi; Yabutani, Tomoki; Okayasu, Takako; Ota, Fusao; Kassu, Afework

    2015-10-01

    Humans and other living organisms require small quantities of trace elements throughout life. Both insufficient and excessive intakes of trace elements can have negative consequences. However, there is little information on serum level of trace elements in different populations. This study examines serum levels of trace elements in Ethiopian, Japanese, and Vietnamese women. Random samples of healthy women who were referred for routine hospital laboratory examinations in the cities of Hanoi, Sapporo, and Gondar were invited to participate in the study. Serum levels of magnesium, zinc, copper, iron, selenium, and calcium were determined using an inductively coupled plasma mass spectrometer. Furthermore, body mass index of each study participant was determined. The mean ± SD serum concentrations of zinc (μg/dL), copper (μg/dL), iron (μg/dL), selenium (μg/dL) and calcium (mg/dL), respectively, were 76.51 ± 39.16, 152.20 ± 55.37, 385.68 ± 217.95, 9.15 ± 4.21, and 14.18 ± 3.91 in Ethiopian women; 111.49 ± 52.92, 105.86 ± 26.02, 155.09 ± 94.83, 14.11 ± 3.41, and 11.66 ± 2.51 in Vietnamese women; and 60.69 ± 9.76, 107 ± 156, 268 ± 128, 8.33 ± 3.65, and 11.18 ± 0.68 in Japanese participants. Ethiopian women had significantly higher level of serum calcium than Vietnamese and Japanese women (both P < 0.05). Although the mean calcium concentration in Vietnamese women was higher than in women from Japan, the difference was not statistically significant (P > 0.05). Furthermore, compared with Japanese women, Ethiopian women had significantly high iron and copper concentrations (P < 0.05). Serum selenium and zinc levels were higher in Vietnamese than Ethiopian women. The study revealed a remarkable difference in serum concentrations of trace elements in women from different countries, implying differences in trace elements in the food or soil. Copyright © 2015 Elsevier Inc. All rights reserved.

  2. Determination of trace metals in spirits by total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Siviero, G.; Cinosi, A.; Monticelli, D.; Seralessandri, L.

    2018-06-01

    Eight spirituous samples were analyzed for trace metal content with Horizon Total Reflection X-Ray Fluorescence (TXRF) Spectrometer. The expected single metal amount is at the ng/g level in a mixed aqueous/organic matrix, thus requiring a sample preparation method capable of achieving suitable limits of detection. On-site enrichment and Atmospheric Pressure-Vapor Phase Decomposition allowed to detect Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Sr and Pb with detection limits ranging from 0.1 ng/g to 4.6 ng/g. These results highlight how the synergy between instrument and sample preparation strategy may foster the use of TXRF as a fast and reliable technique for the determination of trace elements in spirituous samples, either for quality control or risk assessment purposes.

  3. Determination of equivalent sound speed profiles for ray tracing in near-ground sound propagation.

    PubMed

    Prospathopoulos, John M; Voutsinas, Spyros G

    2007-09-01

    The determination of appropriate sound speed profiles in the modeling of near-ground propagation using a ray tracing method is investigated using a ray tracing model which is capable of performing axisymmetric calculations of the sound field around an isolated source. Eigenrays are traced using an iterative procedure which integrates the trajectory equations for each ray launched from the source at a specific direction. The calculation of sound energy losses is made by introducing appropriate coefficients to the equations representing the effect of ground and atmospheric absorption and the interaction with the atmospheric turbulence. The model is validated against analytical and numerical predictions of other methodologies for simple cases, as well as against measurements for nonrefractive atmospheric environments. A systematic investigation for near-ground propagation in downward and upward refractive atmosphere is made using experimental data. Guidelines for the suitable simulation of the wind velocity profile are derived by correlating predictions with measurements.

  4. Sample preparation techniques for the determination of trace residues and contaminants in foods.

    PubMed

    Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

    2007-06-15

    The determination of trace residues and contaminants in complex matrices, such as food, often requires extensive sample extraction and preparation prior to instrumental analysis. Sample preparation is often the bottleneck in analysis and there is a need to minimise the number of steps to reduce both time and sources of error. There is also a move towards more environmentally friendly techniques, which use less solvent and smaller sample sizes. Smaller sample size becomes important when dealing with real life problems, such as consumer complaints and alleged chemical contamination. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This review considers all aspects of sample preparation, covering general extraction techniques, such as Soxhlet and pressurised liquid extraction, microextraction techniques such as liquid phase microextraction (LPME) and more selective techniques, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The applicability of each technique in food analysis, particularly for the determination of trace organic contaminants in foods is discussed.

  5. Determining Hypocentral Parameters for Local Earthquakes in 1-D Using a Genetic Algorithm and Two-point ray tracing

    NASA Astrophysics Data System (ADS)

    Kim, W.; Hahm, I.; Ahn, S. J.; Lim, D. H.

    2005-12-01

    This paper introduces a powerful method for determining hypocentral parameters for local earthquakes in 1-D using a genetic algorithm (GA) and two-point ray tracing. Using existing algorithms to determine hypocentral parameters is difficult, because these parameters can vary based on initial velocity models. We developed a new method to solve this problem by applying a GA to an existing algorithm, HYPO-71 (Lee and Larh, 1975). The original HYPO-71 algorithm was modified by applying two-point ray tracing and a weighting factor with respect to the takeoff angle at the source to reduce errors from the ray path and hypocenter depth. Artificial data, without error, were generated by computer using two-point ray tracing in a true model, in which velocity structure and hypocentral parameters were known. The accuracy of the calculated results was easily determined by comparing calculated and actual values. We examined the accuracy of this method for several cases by changing the true and modeled layer numbers and thicknesses. The computational results show that this method determines nearly exact hypocentral parameters without depending on initial velocity models. Furthermore, accurate and nearly unique hypocentral parameters were obtained, although the number of modeled layers and thicknesses differed from those in the true model. Therefore, this method can be a useful tool for determining hypocentral parameters in regions where reliable local velocity values are unknown. This method also provides the basic a priori information for 3-D studies. KEY -WORDS: hypocentral parameters, genetic algorithm (GA), two-point ray tracing

  6. Ultra-performance liquid chromatographic determination of L-ergothioneine in commercially available classes of cow milk.

    PubMed

    Sotgia, Salvatore; Pisanu, Elisabetta; Cambedda, Debora; Pintus, Gianfranco; Carru, Ciriaco; Zinellu, Angelo

    2014-09-01

    A new efficient and sensitive precolumn hydrophilic interaction ultra-performance liquid chromatography (HILIC-UPLC) method was established for the quantitative determination of L-ergothioneine (ERT) in milk. After derivatization of ERT with 7-diethylamino-3-[4-(iodoacetamido)phenyl]-4-methylcoumarin, chromatographic separation was achieved in a fairly short time, less than 5 min, on a 100 × 2.1 mm Waters Cortecs UPLC HILIC 1.6-μm column, by using a mixture of 30 mmol/L ammonium acetate/acetonitrile (10:90, v/v) as a mobile phase flowing isocratically at 0.9 mL/min. Limit of detection and the limit of quantification were 0.03 and 0.10 μmol/L, respectively. The method exhibited linearity in a concentration range of 0.16 and 5.08 μmol/L. Mean recovery was 106.66%, whereas intra- and interassay precisions were determined to be within 6 RSD%. On average, ERT concentration in different commercially available classes of cow milk was found to be 0.442 ± 0.191 μmol/L, with the highest levels in the ultra-high temperature milks and low values in the unprocessed and HTST whole milks. In this light, our experiments suggest that ERT could be used as a marker for the heat treatment of milk. © 2014 Institute of Food Technologists®

  7. Determination of Trace Deoxyribonucleic Acid by Using Fluorescein Isothiocyanate-Phenosafranine as a Double-Luminescent Phosphorescence Probe

    PubMed Central

    Huang, Xiao-Mei; Liu, Zhen-Bo; Li, Fei-Ming; Lin, Li-Ping; Wang, Xin-Xing; Lin, Chang-Qing; Huang, Ya-Hong; Li, Zhi-Ming; Lin, Shao-Qin

    2010-01-01

    Using Pb2+ as ion perturber, phenosafranine (PF) and fluorescein isothiocyanate (FITC) could emit strong and stable room temperature phosphorescence (RTP) signal on the filter paper, respectively. When they were mixed, the phenomenon that the RTP signal of PF and FITC enhanced significantly was found. And 1.12 ag DNA spot−1 (sample volume was 0.40 μL, corresponding concentration was 2.8 × 10–15 g mL–1) could cause the RTP signal of both PF and FITC to enhance sharply. The content of DNA was proportional to the ΔIp of PF and FITC in the system at 634 and 659 nm. Thus, a new solid substrate room temperature phosphorimetry (SSRTP) for the determination of trace DNA was established by using FITC-PF as double-luminescent phosphorescence probe. The detection limit (LD) of this method calculated by 3Sb/k was 14 zg DNA spot–1 for PF and 18 zg DNA spot–1 for FITC, respectively, showing high sensitivity. It has been applied to the determination of trace DNA in practical samples and the analysis results were in accordance with those of fluorescence probe. The reaction mechanism of SSRTP for the determination of trace DNA was also discussed. PMID:20665096

  8. Study of carbon nanotube-rich impedimetric recognition electrode for ultra-low determination of polycyclic aromatic hydrocarbons in water.

    PubMed

    Muñoz, Jose; Navarro-Senent, Cristina; Crivillers, Nuria; Mas-Torrent, Marta

    2018-04-14

    Carbon nanotubes (CNTs) have been studied as an electrochemical recognition element for the impedimetric determination of priority polycyclic aromatic hydrocarbons (PAHs) in water, using hexocyanoferrate as a redox probe. For this goal, an indium tin oxide (ITO) electrode functionalized with a silane-based self-assembled monolayer carrying CNTs has been engineered. The electroanalytical method, which is similar to an antibody-antigen assay, is straightforward and exploits the high CNT-PAH affinity obtained via π-interactions. After optimizing the experimental conditions, the resulting CNT-based impedimetric recognition platform exhibits ultra-low detection limits (1.75 ± 0.04 ng·L -1 ) for the sum of PAHs tested, which was also validated by using a certified reference PAH mixture. Graphical abstract Schematic of an indium-tin-oxide (ITO) electrode functionalized with a silane-based self-assembled monolayer carrying carbon nanotubes (CNTs) as a recognition platform for the ultra-low determination of total polycyclic aromatic hydrocarbons (PAHs) in water via π-interactions using Electrochemical Impedance Spectroscopy (EIS).

  9. Trace element determination using static high-sensitivity inductively coupled plasma optical emission spectrometry (SHIP-OES).

    PubMed

    Engelhard, Carsten; Scheffer, Andy; Nowak, Sascha; Vielhaber, Torsten; Buscher, Wolfgang

    2007-02-05

    A low-flow air-cooled inductively coupled plasma (ICP) design for optical emission spectrometry (OES) with axial plasma viewing is described and an evaluation of its analytical capabilities in trace element determinations is presented. Main advantage is a total argon consumption of 0.6 L min(-1) in contrast to 15 L min(-1) using conventional ICP sources. The torch was evaluated in trace element determinations and studied in direct comparison with a conventional torch under the same conditions with the same OES system, ultrasonic nebulization (USN) and single-element optimization. A variety of parameters (x-y-position of the torch, rf power, external air cooling, gas flow rates and USN operation parameters) was optimized to achieve limits of detection (LOD) which are competitive to those of a conventional plasma source. Ionic to atomic line intensity ratios for magnesium were studied at different radio frequency (rf) power conditions and different sample carrier gas flows to characterize the robustness of the excitation source. A linear dynamic range of three to five orders of magnitude was determined under compromise conditions in multi-element mode. The accuracy of the system was investigated by the determination of Co, Cr, Mn, Zn in two certified reference materials (CRM): CRM 075c (Copper with added impurities), and CRM 281 (Trace elements in rye grass). With standard addition values of 2.44+/-0.04 and 3.19+/-0.21 microg g(-1) for Co and Mn in the CRM 075c and 2.32+/-0.09, 81.8+/-0.4, 32.2+/-3.9 for Cr, Mn and Zn, respectively, were determined in the samples and found to be in good agreement with the reported values; recovery rates in the 98-108% range were obtained. No influence on the analysis by the matrix load in the sample was observed.

  10. Rapid determination of quinolones in cosmetic products by ultra high performance liquid chromatography with tandem mass spectrometry.

    PubMed

    Liu, Shao-Ying; Huang, Xi-Hui; Wang, Xiao-Fang; Jin, Quan; Zhu, Guo-Nian

    2014-05-01

    This study developed an improved analytical method for the simultaneous quantification of 13 quinolones in cosmetics by ultra high performance liquid chromatography combined with ESI triple quadrupole MS/MS under the multiple reaction monitoring mode. The analytes were extracted and purified by using an SPE cartridge. The limits of quantification ranged from 0.03 to 3.02 μg/kg. The precision for determining the quinolones was <19.39%. The proposed method was successfully developed for the determination of quinolones in real cosmetic samples. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. New trace element determinations in the fingernails of ALS patients

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

    Van Dalsem, D.J.; Ehmann, W.D.; Robinson, L.

    1996-12-31

    Amyotrophic lateral sclerosis (ALS) afflicts 2 of every 100,000 people in the United States each year. A well-known example of ALS today is Stephen Hawking. He is a theoretical physicist, the author of A Brief History of Time, and is virtually immobilized by ALS. Diseases that cause progressive paralysis because of motor neuron degeneration in the central nervous system are termed motor neuron disorders (MND). Amyotrophic lateral sclerosis is a common form of MND. Pain-free, progressive muscular weakness is the most common clinical symptom. There is chronic weakness with atrophy of the affected muscles by the time the disease ismore » diagnosed. Atrophy eventually results in wheelchair confinement and then only bed without the ability to speak or swallow. Death often occurs as a result of respiratory problems. Unlike other neurodegenerative diseases, in ALS the patient`s bladder and bowel control, eye movement, and mental faculties are preserved. The question today is whether or not certain trace elements are involved in the etiology or pathogenesis of ALS. A collaborative study was undertaken by the University of Kentucky and Oak Ridge National Laboratory (ORNL) using neutron activation analysis (NAA) to study trace element concentrations in ALS patients fingernails to determine if there existed statistically significant imbalances.« less

  12. Determination of 2-alkylcyclobutanones by combining precolumn derivatization with 1-naphthalenyl hydrazine and ultra-performance liquid chromatography with fluorescence detection.

    PubMed

    Meng, Xiangpeng; Tong, Tong; Wang, Lianrong; Liu, Hanxia; Chan, Wan

    2016-05-01

    2-Alkylcyclobutanones (2-ACBs) are uniquely formed when triglycerides-containing food products are exposed to ionizing radiation. Thus, 2-ACBs have been used as marker molecules to identify irradiated food. Most methods to determine 2-ACBs involve mass spectrometric detection after chromatographic separation. The spectrofluorometer is rarely used to determine 2-ACBs because these molecules do not fluoresce. In this study, we developed an ultra-performance liquid chromatography (UPLC) method to determine 2-ACBs. 2-ACBs were converted into fluorophores after reacting with 1-naphthalenyl hydrazine to facilitate their sensitive and selective detection using a fluorescence detector (FLD). Analysis of 2-ACBs using our developed UPLC-FLD method allows sensitive determination of 2-ACBs at a detection limit of 2 ng 2-ACBs per g of fat (30 pg/injection), which is significantly lower than that of existing analytical methods. After validation for trueness and precision, the method was applied to γ-irradiated chicken samples to determine their 2-ACB content. Comparative studies employing liquid chromatography-tandem mass spectrometric method revealed no systematic difference between the two methods, thereby demonstrating that the proposed UPLC-FLD method can be suitably used to determine 2-ACBs in irradiated foodstuffs. Graphical Abstract Determination of radiation-induced food-borne 2-dodecylcyclobutanone and 2-tetradecylcyclobutanone by combining 1-naphthalenyl hydrazine derivatization and ultra-performance liquid chromatography with fluorescence detection.

  13. Determination of dasatinib in the tablet dosage form by ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis.

    PubMed

    Gonzalez, Aroa Garcia; Taraba, Lukáš; Hraníček, Jakub; Kozlík, Petr; Coufal, Pavel

    2017-01-01

    Dasatinib is a novel oral prescription drug proposed for treating adult patients with chronic myeloid leukemia. Three analytical methods, namely ultra high performance liquid chromatography, capillary zone electrophoresis, and sequential injection analysis, were developed, validated, and compared for determination of the drug in the tablet dosage form. The total analysis time of optimized ultra high performance liquid chromatography and capillary zone electrophoresis methods was 2.0 and 2.2 min, respectively. Direct ultraviolet detection with detection wavelength of 322 nm was employed in both cases. The optimized sequential injection analysis method was based on spectrophotometric detection of dasatinib after a simple colorimetric reaction with folin ciocalteau reagent forming a blue-colored complex with an absorbance maximum at 745 nm. The total analysis time was 2.5 min. The ultra high performance liquid chromatography method provided the lowest detection and quantitation limits and the most precise and accurate results. All three newly developed methods were demonstrated to be specific, linear, sensitive, precise, and accurate, providing results satisfactorily meeting the requirements of the pharmaceutical industry, and can be employed for the routine determination of the active pharmaceutical ingredient in the tablet dosage form. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Ultra-sensitive all-fibre photothermal spectroscopy with large dynamic range

    PubMed Central

    Jin, Wei; Cao, Yingchun; Yang, Fan; Ho, Hoi Lut

    2015-01-01

    Photothermal interferometry is an ultra-sensitive spectroscopic means for trace chemical detection in gas- and liquid-phase materials. Previous photothermal interferometry systems used free-space optics and have limitations in efficiency of light–matter interaction, size and optical alignment, and integration into photonic circuits. Here we exploit photothermal-induced phase change in a gas-filled hollow-core photonic bandgap fibre, and demonstrate an all-fibre acetylene gas sensor with a noise equivalent concentration of 2 p.p.b. (2.3 × 10−9 cm−1 in absorption coefficient) and an unprecedented dynamic range of nearly six orders of magnitude. The realization of photothermal interferometry with low-cost near infrared semiconductor lasers and fibre-based technology allows a class of optical sensors with compact size, ultra sensitivity and selectivity, applicability to harsh environment, and capability for remote and multiplexed multi-point detection and distributed sensing. PMID:25866015

  15. Determination of Trace Level Iodine in Biological and Botanical Reference Materials by Isotope Dilution Mass Spectrometry

    PubMed Central

    Gramlich, John W.; Murphy, Thomas J.

    1989-01-01

    A method has been developed for the determination of trace level iodine in biological and botanical materials. The method consists of spiking a sample with 129I, equilibration of the spike with the natural iodine, wet ashing under carefully controlled conditions, and separation of the iodine by co-precipitation with silver chloride. Measurement of the 129I/127I ratio is accomplished by negative thermal ionization mass spectrometry using LaB6 for ionization enhancement. The application of the method to the certification of trace iodine in two Standard Reference Materials is described. PMID:28053411

  16. Rhabdomyolysis and exercise-associated hyponatremia in ultra-bikers and ultra-runners.

    PubMed

    Chlíbková, Daniela; Knechtle, Beat; Rosemann, Thomas; Tomášková, Ivana; Novotný, Jan; Žákovská, Alena; Uher, Tomáš

    2015-01-01

    Exercise-associated hyponatremia (EAH), rhabdomyolysis and renal failure appear to be a unique problem in ultra-endurance racers. We investigated the combined occurrence of EAH and rhabdomyolysis in seven different ultra-endurance races and disciplines (i.e. multi-stage mountain biking, 24-h mountain biking, 24-h ultra-running and 100-km ultra-running). Two (15.4%) ultra-runners (man and woman) from hyponatremic ultra-athletes (n = 13) and four (4%) ultra-runners (four men) from the normonatremic group (n = 100) showed rhabdomyolysis following elevated blood creatine kinase (CK) levels > 10,000 U/L without the development of renal failure and the necessity of a medical treatment. Post-race creatine kinase, plasma and urine creatinine significantly increased, while plasma [Na(+)] and creatine clearance decreased in hyponatremic and normonatremic athletes, respectively. The percentage increase of CK was higher in the hyponatremic compared to the normonatremic group (P < 0.05). Post-race CK levels were higher in ultra-runners compared to mountain bikers (P < 0.01), in faster normonatremic (P < 0.05) and older and more experienced hyponatremic ultra-athletes (P < 0.05). In all finishers, pre-race plasma [K(+)] was related to post-race CK (P < 0.05). Hyponatremic ultra-athletes tended to develop exercise-induced rhabdomyolysis more frequently than normonatremic ultra-athletes. Ultra-runners tended to develop rhabdomyolysis more frequently than mountain bikers. We found no association between post-race plasma [Na(+)] and CK concentration in both hypo- and normonatremic ultra-athletes.

  17. An Ultra-Trace Analysis Technique for SF6 Using Gas Chromatography with Negative Ion Chemical Ionization Mass Spectrometry.

    PubMed

    Jong, Edmund C; Macek, Paul V; Perera, Inoka E; Luxbacher, Kray D; McNair, Harold M

    2015-07-01

    Sulfur hexafluoride (SF6) is widely used as a tracer gas because of its detectability at low concentrations. This attribute of SF6 allows the quantification of both small-scale flows, such as leakage, and large-scale flows, such as atmospheric currents. SF6's high detection sensitivity also facilitates greater usage efficiency and lower operating cost for tracer deployments by reducing quantity requirements. The detectability of SF6 is produced by its high molecular electronegativity. This property provides a high potential for negative ion formation through electron capture thus naturally translating to selective detection using negative ion chemical ionization mass spectrometry (NCI-MS). This paper investigates the potential of using gas chromatography (GC) with NCI-MS for the detection of SF6. The experimental parameters for an ultra-trace SF6 detection method utilizing minimal customizations of the analytical instrument are detailed. A method for the detection of parts per trillion (ppt) level concentrations of SF6 for the purpose of underground ventilation tracer gas analysis was successfully developed in this study. The method utilized a Shimadzu gas chromatography with negative ion chemical ionization mass spectrometry system equipped with an Agilent J&W HP-porous layer open tubular column coated with an alumina oxide (Al2O3) S column. The method detection limit (MDL) analysis as defined by the Environmental Protection Agency of the tracer data showed the method MDL to be 5.2 ppt. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  18. [Ultra-Fine Pressed Powder Pellet Sample Preparation XRF Determination of Multi-Elements and Carbon Dioxide in Carbonate].

    PubMed

    Li, Xiao-li; An, Shu-qing; Xu, Tie-min; Liu, Yi-bo; Zhang, Li-juan; Zeng, Jiang-ping; Wang, Na

    2015-06-01

    The main analysis error of pressed powder pellet of carbonate comes from particle-size effect and mineral effect. So in the article in order to eliminate the particle-size effect, the ultrafine pressed powder pellet sample preparation is used to the determination of multi-elements and carbon-dioxide in carbonate. To prepare the ultrafine powder the FRITSCH planetary Micro Mill machine and tungsten carbide media is utilized. To conquer the conglomeration during the process of grinding, the wet grinding is preferred. The surface morphology of the pellet is more smooth and neat, the Compton scatter effect is reduced with the decrease in particle size. The intensity of the spectral line is varied with the change of the particle size, generally the intensity of the spectral line is increased with the decrease in the particle size. But when the particle size of more than one component of the material is decreased, the intensity of the spectral line may increase for S, Si, Mg, or decrease for Ca, Al, Ti, K, which depend on the respective mass absorption coefficient . The change of the composition of the phase with milling is also researched. The incident depth of respective element is given from theoretical calculation. When the sample is grounded to the particle size of less than the penetration depth of all the analyte, the effect of the particle size on the intensity of the spectral line is much reduced. In the experiment, when grounded the sample to less than 8 μm(d95), the particle-size effect is much eliminated, with the correction method of theoretical α coefficient and the empirical coefficient, 14 major, minor and trace element in the carbonate can be determined accurately. And the precision of the method is much improved with RSD < 2%, except Na2O. Carbon is ultra-light element, the fluorescence yield is low and the interference is serious. With the manual multi-layer crystal PX4, coarse collimator, empirical correction, X-ray spectrometer can be used to

  19. In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

    PubMed

    Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

    2018-03-01

    In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

  20. Semiautomated determination of neonicotinoids and characteristic metabolite in urine samples using TurboFlow™ coupled to ultra high performance liquid chromatography coupled to Orbitrap analyzer.

    PubMed

    López-García, Marina; Romero-González, Roberto; Lacasaña, Marina; Garrido Frenich, Antonia

    2017-11-30

    A semiautomated method based on ultra-high performance liquid chromatography (UHPLC) coupled to Orbitrap high resolution mass spectrometry has been developed for the determination of neonicotinoids (imidacloprid, acetamiprid, clothianidin, dinotefuran, nitenpyram, thiacloprid and thiamethoxam) and the metabolite acetamiprid-n-desmethyl in urine samples. Two automated methods were tested (solid-phase extraction "SPE" and turbulent flow chromatography "TurboFlow™"), obtaining the best results when TurboFlow™ was applied. The total analysis time for the developed method was 14min. The optimized method was validated, obtaining suitable results for all validation parameters. Recoveries ranged from 78% to 116% meanwhile repeatability and reproducibility were evaluated obtaining values lower than 10% and 20% respectively (except for dinotefuran and nitenpyram at 0.2μgL -1 ). The limit of quantification (LOQ) for all compounds was established at 0.2μgL -1 . The proposed analytical methodology was applied to analyze the target compounds in thirty six urine samples from pregnant women living in agricultural areas of Almería (Spain). Imidacloprid, acetamiprid and acetamiprid-n-desmethyl were detected in some of the samples at concentrations ranging from 0.23 to 1.57μgL -1 . Furthermore, dinotefuran was identified in two samples at trace levels. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Immunoaffinity column as clean-up tool for determination of trace amounts of microcystins in tap water.

    PubMed

    Tsutsumi, T; Nagata, S; Hasegawa, A; Ueno, Y

    2000-07-01

    Trace amounts of microcystins (MCs) in drinking water should be monitored because of their potential hazard for human health as an environmental tumor promoter. We describe here a new clean-up tool with immunoaffinity column (IAC) for determination of trace amounts of MCs (from pg to microg/litre) in tap water. The water samples were concentrated with IAC clean-up and MCs levels were determined by HPLC with UV detection or enzyme-linked immunosorbent assay (ELISA). In the combination with HPLC analysis, mean recovery of microcystin-LR (MCLR),-RR and-YR spiked to tap water were 91.8%, 77.3% and 86.4%, respectively, in the range 2.5-100 microg/litre. The chromatogram of MCs-spiked tap water sample cleaned up with IAC showed effective elimination of the impurities compared to that with octadecyl silanized cartridge, which had been cleaned up with a conventional method. Also, in the combination with highly sensitive ELISA, mean recovery of MCLR spiked to tap water was 80% in the range 0.1-1000 ng/litre. The combined methods developed here can detect pg to microg/litre of MCs in tap water. The overall results indicated that IAC will be suitable as a clean-up tool for trace amounts of MCs in tap water.

  2. THE DETERMINATION OF TRACES OF IRON IN SAMPLES OF PLATINUM BY NE TRON- ACTIVATION ANALYSIS

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

    Morris, D.F.C.; Killick, R.A.

    1963-11-01

    A neutron-activation analysis method for the determination of traces of iron in samples of purified platinum is described. The nuclear reactor BEPO at Harwell was used as the neutron source. A rapid radiochemical separation procedure using carriers was employed to decontaminate the iron activity from most other induced activities. The analysis is completed by discriminated gamma scintillation counting. Results of analyses of seven samples of platinum are quoted. The method of analysis has the advantage that it obviates difficulties caused by reagent blanks or by contamination from traces of inactive iron after irradiation. Interference resulting from nuclear reactions of elementsmore » other than iron in the samples appears to be of no consequence. (auth)« less

  3. Microwave assisted digestion followed by ICP-MS for determination of trace metals in atmospheric and lake ecosystem.

    PubMed

    Ahmed, Manan; Chin, Ying Hui; Guo, Xinxin; Zhao, Xing-Min

    2017-05-01

    The study of trace metals in the atmosphere and lake water is important due to their critical effects on humans, aquatic animals and the geochemical balance of ecosystems. The objective of this study was to investigate the concentration of trace metals in atmospheric and lake water samples during the rainy season (before and after precipitation) between November and December 2015. Typical methods of sample preparation for trace metal determination such as cloud point extraction, solid phase extraction and dispersive liquid-liquid micro-extraction are time-consuming and difficult to perform; therefore, there is a crucial need for development of more effective sample preparation procedure. A convection microwave assisted digestion procedure for extraction of trace metals was developed for use prior to inductively couple plasma-mass spectrometric determination. The result showed that metals like zinc (133.50-419.30μg/m 3 ) and aluminum (53.58-378.93μg/m 3 ) had higher concentrations in atmospheric samples as compared to lake samples before precipitation. On the other hand, the concentrations of zinc, aluminum, chromium and arsenic were significantly higher in lake samples after precipitation and lower in atmospheric samples. The relationship between physicochemical parameters (pH and turbidity) and heavy metal concentrations was investigated as well. Furthermore, enrichment factor analysis indicated that anthropogenic sources such as soil dust, biomass burning and fuel combustion influenced the metal concentrations in the atmosphere. Copyright © 2016. Published by Elsevier B.V.

  4. Determination of trace amounts of tin in geological materials by atomic absorption spectrometry

    USGS Publications Warehouse

    Welsch, E.P.; Chao, T.T.

    1976-01-01

    An atomic absorption method is described for the determination of traces of tin in rocks, soils, and stream sediments. A dried mixture of the sample and ammonium iodide is heated to volatilize tin tetraiodide -which is then dissolved in 5 % hydrochloric acid, extracted into TOPO-MIBK, and aspirated into a nitrous oxide-acetylene flame. The limit of determination is 2 p.p.m. tin and the relative standard deviation ranges from 2 to 14 %. Up to 20 % iron and 1000 p.p.m. Cu, Pb, Zn, Mn, Hg, Mo, V, or W in the sample do not interfere. As many as 50 samples can be easily analyzed per man-day. ?? 1976.

  5. Solvent extraction of oil-sand components for determination of trace elements by neutron activation analysis

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

    Jacobs, F.S.; Filby, R.H.

    Instrumental neutron activation analysis was used to measure the concentrations of 30 elements in Athabasca oil sands and oil-sand components. The oil sands were separated into solid residue, bitumen, and fines by Soxhlet extraction with toluene-bitumen extract. The mineral content of the extracted bitumen was dependent on the treatment of the oil sand prior to extraction. The geochemically important and organically associated trace element contents of the bitumen (and asphaltenes) were determined by subtracting the mineral contributions from the total measured concentrations. The method allows analysis of the bitumen without the necessity of ultracentrifugation or membrane filtration, which might removemore » geochemically important components of the bitumen. The method permits classification of trace elements into organic and inorganic combinations.« less

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

    PubMed

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

    2011-01-01

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

  7. Catalytic solid substrate room temperature phosphorimetry for the determination of trace rhamnose based on its condensation reaction with calcein

    NASA Astrophysics Data System (ADS)

    Liu, Jia-Ming; Lin, Li-Ping; Wang, Hong-Xin; Lin, Shao-Qin; Zhang, Li-Hong; Cai, Wen-Lian; Lin, Xuan; Pan, You-Zhu; Wang, Xin-Xing; Li, Zhi-Ming; Jiao, Li; Cui, Ma-Lin

    2011-12-01

    Calcein (R) could not only emit strong and stable room temperature phosphorescence (RTP) on filter paper using I - as perturber, but also could be oxidized by H 2O 2 to form a non-phosphorescence compound (R'), resulting in the quenching of RTP signal of R. Moreover, the ortho-hydrogen of phenolic hydroxyl in R took condensation reaction with rhamnose (Rha) to produce non-phosphorescence compound (R-Rha) causing the RTP signal of R to further quench, and R-Rha was oxidized by H 2O 2 to form R' and Rha, bringing about the sharp RTP signal quenching of R. Thus, a new solid substrate room temperature phosphorimetry (SSRTP) for the determination of trace Rha based on its strong catalytic effect on H 2O 2 oxidizing R has been established, with the detection limit (LD) of 7.8 zg spot -1 (corresponding concentration: 2.0 × 10 -17 g ml -1, sample volume: 0.40 μl spot -1). This method has been applied to determine trace Rha in cigarettes and jujubes, with the results coinciding well with those determined by a high performance liquid chromatography (HPLC). The component of R-Rha also was analyzed by means of HPLC, mass spectrometer and nuclear magnetic resonance (NMR) measurements. The mechanism of catalytic SSRTP for the determination of trace Rha was discussed.

  8. Determination of caramel colorants' by-products in liquid foods by ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).

    PubMed

    Goscinny, Séverine; Hanot, Vincent; Trabelsi, Hasna; Van Loco, Joris

    2014-01-01

    2-Methylimidazole, 4-methylimidazole (2-MI and 4-MI), 2-acetyl-4-(1,2,3,4-tetrahydroxybutyl) imidazole (THI) and 5-hydroxymethylfurfural (5-HMF) are neo-formed compounds generated during the manufacture of caramel colours and are transferred to the processed food. These contaminants are known to have a toxicological profile that may pose health risks. Hence, to characterise THI, 2- and 4-MI and 5-HMF levels in liquid foods, an ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and sample preparation was divided into two analytical strategies depending on the concentration range expected in the type of foods targeted. For the determination of the imidazole substitutes (THI, 2- and 4-MI), a sample enrichment and clean-up step by strong cation solid-phase extraction was developed. This method is capable of quantifying over a range of 5 ng ml⁻¹ (LOQ) to 500 ng ml⁻¹ with recoveries of 75.4-112.4% and RSDs of 1.5-15%. For determination of 5-HMF, a standard addition method was applied covering the linear range of 0.25-30 µg ml⁻¹ with RSDs from 2.8% (for intraday precision) to 9.2% (for intermediate precision). The validated analytical methods were applied to 28 liquid food samples purchased from local markets. THI was found only in the beer samples at levels up to 141.2 ng ml⁻¹. For 2-MI, non-quantifiable traces were observed for all samples, while 4-MI was observed in all samples with large concentration variations (from < LOQ to 563.9 ng ml⁻¹). 5-HMF was found at expected concentrations, except for a sherry vinegar sample (113 µg ml⁻¹), which required a high level of dilution before following the standard addition protocol.

  9. Ionic liquid-based extraction followed by graphite-furnace atomic absorption spectrometry for the determination of trace heavy metals in high-purity iron metal.

    PubMed

    Matsumiya, Hiroaki; Kato, Tatsuya; Hiraide, Masataka

    2014-02-01

    The analysis of high-purity materials for trace impurities is an important and challenging task. The present paper describes a facile and sensitive method for the determination of trace heavy metals in high-purity iron metal. Trace heavy metals in an iron sample solution were rapidly and selectively preconcentrated by the extraction into a tiny volume of an ionic liquid [1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide] for the determination by graphite-furnace atomic absorption spectrometry (GFAAS). A nitrogen-donating neutral ligand, 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ), was found to be effective in the ionic liquid-based selective extraction, allowing the nearly complete (~99.8%) elimination of the iron matrix. The combination with the optimized GFAAS was successful. The detectability reached sub-μg g(-1) levels in iron metal. The novel use of TPTZ in ionic liquid-based extraction followed by GFAAS was successfully applied to the determination of traces of Co, Ni, Cu, Cd, and Pb in certified reference materials for high-purity iron metal. © 2013 Published by Elsevier B.V.

  10. Compositional variations at ultra-structure length scales in coral skeleton

    NASA Astrophysics Data System (ADS)

    Meibom, Anders; Cuif, Jean-Pierre; Houlbreque, Fanny; Mostefaoui, Smail; Dauphin, Yannicke; Meibom, Karin L.; Dunbar, Robert

    2008-03-01

    Distributions of Mg and Sr in the skeletons of a deep-sea coral ( Caryophyllia ambrosia) and a shallow-water, reef-building coral ( Pavona clavus) have been obtained with a spatial resolution of 150 nm, using the NanoSIMS ion microprobe at the Muséum National d'Histoire Naturelle in Paris. These trace element analyses focus on the two primary ultra-structural components in the skeleton: centers of calcification (COC) and fibrous aragonite. In fibrous aragonite, the trace element variations are typically on the order of 10% or more, on length scales on the order of 1-10 μm. Sr/Ca and Mg/Ca variations are not correlated. However, Mg/Ca variations in Pavona are strongly correlated with the layered organization of the skeleton. These data allow for a direct comparison of trace element variations in zooxanthellate and non-zooxanthellate corals. In both corals, all trace elements show variations far beyond what can be attributed to variations in the marine environment. Furthermore, the observed trace element variations in the fibrous (bulk) part of the skeletons are not related to the activity of zooxanthellae, but result from other biological activity in the coral organism. To a large degree, this biological forcing is independent of the ambient marine environment, which is essentially constant on the growth timescales considered here. Finally, we discuss the possible detection of a new high-Mg calcium carbonate phase, which appears to be present in both deep-sea and reef-building corals and is neither aragonite nor calcite.

  11. Simultaneous speciation and preconcentration of ultra traces of inorganic tellurium and selenium in environmental samples by hollow fiber liquid phase microextraction prior to electrothermal atomic absorption spectroscopy determination.

    PubMed

    Ghasemi, Ensieh; Najafi, Nahid Mashkouri; Raofie, Farhad; Ghassempour, Alireza

    2010-09-15

    A simple and effective speciation and preconcentration method based on hollow fiber liquid phase microextraction (HF-LPME) was developed for simultaneous separation of trace inorganic tellurium and selenium in environmental samples prior to electrothermal atomic absorption spectroscopy (ETAAS) determination. The method involves the selective extraction of the Te (IV) and Se (IV) species by HF-LPME with the use of ammonium pyrrolidinecarbodithioate (APDC) as the chelating agent. The complex compounds were extracted into 10 microL of toluene and the solutions were injected into a graphite furnace for the determination of Te (IV) and Se (IV). To determine the total tellurium and selenium in the samples, first Te (VI) and Se (VI) were reduced to Te (IV) and Se (IV), and then the microextraction method was performed. The experimental parameters of HF-LPME were optimized using a central composite design after a 2(n-1) fractional factorial experimental design. Under optimum conditions, enrichment factors of up to 520 and 480 were achieved for Te (IV) and Se (IV), respectively. The detection limits were 4 ng L(-1) with 3.5% RSD (n=5, c=2.0 microg L(-1)) for Te (IV) and 5 ng L(-1) with 3.1% RSD for Se (IV). The applicability of the developed technique was evaluated by application to spiked, environmental water and soil samples. Copyright 2010 Elsevier B.V. All rights reserved.

  12. (F)UV Spectroscopy of K648: Abundance Determination of Trace Elements

    NASA Astrophysics Data System (ADS)

    Mohamad-Yob, S. J.; Ziegler, M.; Rauch, T.; Werner, K.

    2010-11-01

    We present preliminary results of an ongoing spectral analysis of K 648, the central star of the planetary nebula Ps 1, based on high resolution FUV spectra. K 648, in M 15 is one of only four known PNe in globular clusters. The formation of this post-AGB object in a globular cluster is still unclear. Our aim is to determine Teff, log g, and the abundances of trace elements, in order to improve our understanding of post-AGB evolution of extremely metal-poor stars, especially PN formation in globular clusters. We analyzed FUSE, HST/STIS, and HST/FOS observations. A grid of stellar model atmospheres was calculated using the Tübingen NLTE Model Atmosphere Package (TMAP).

  13. Few-cycle pulse laser induced damage threshold determination of ultra-broadband optics.

    PubMed

    Kafka, Kyle R P; Talisa, Noah; Tempea, Gabriel; Austin, Drake R; Neacsu, Catalin; Chowdhury, Enam A

    2016-12-12

    A systematic study of few-cycle pulse laser induced damage threshold (LIDT) determination was performed for commercially-available ultra-broadband optics, (i.e. chirped mirrors, silver mirrors, beamsplitters, etc.) in vacuum and in air, for single and multi-pulse regime (S-on-1). Multi-pulse damage morphology at fluences below the single-pulse LIDT was studied in order to investigate the mechanisms leading to the onset of damage. Stark morphological contrast was observed between multi-pulse damage sites formed in air versus those in vacuum. One effect of vacuum testing compared to air included suppression of laser-induced periodic surface structures (LIPSS) formation, possibly influenced by a reduced presence of damage debris. Another effect of vacuum was occasional lowering of LIDT, which appears to be due to the stress-strain performance of the coating design during laser irradiation and under the external stress of vacuum ambience. A fused silica substrate is also examined, and a non-LIPSS nanostructuring is observed on the surface. Possible mechanisms are discussed.

  14. Simultaneous determination of four alkaloids in Lindera aggregata by ultra-high-pressure liquid chromatography-tandem mass spectrometry.

    PubMed

    Han, Zheng; Zheng, Yunliang; Chen, Na; Luan, Lianjun; Zhou, Changxin; Gan, Lishe; Wu, Yongjiang

    2008-11-28

    A new separation and quantification method using liquid chromatography under ultra-high-pressure in combination with tandem mass spectrometry (MS/MS) was developed for simultaneous determination of four alkaloids in Lindera aggregata. The analysis was performed on an Acquity UPLC BEH C(18) column (50mmx2.1mm, 1.7microm particle size; Waters, Milford, MA, USA) utilizing a gradient elution profile and a mobile phase consisting of (A) water containing 10mM ammonium acetate adjusted to pH 3 with acetic acid and (B) acetonitrile. An electrospray ionization (ESI)-tandem interface in the positive mode was employed prior to mass spectrometric detection. The calibration curve was linear over the range of 17.1-856ng for boldine, 42.4-2652ng for norboldine, 6.1-304ng for reticuline and 0.5-50ng for linderegatine, respectively. The average recoveries ranged from 99.2 to 101.4% with RSDs< or =2.7%. Then, four L. aggregata samples from different batches were analyzed using the established method. The results indicated that ultra-high-pressure liquid chromatography-tandem mass spectrometry provided improved chromatographic parameters resulting in significantly increased sample throughput including lower solvent consumption and lower limits of quantitation (LOQs) for most of target analytes compared to previous method employing conventional high-performance liquid chromatography (HPLC) separation. So, the established method was validated, sensitive and reliable for the determination of four alkaloids in L. aggregata.

  15. Detection of vehicle-based improvised explosives using ultra-trace detection equipment

    NASA Astrophysics Data System (ADS)

    Fisher, Mark; Sikes, John; Prather, Mark; Wichert, Clint

    2005-05-01

    Vehicle-borne improvised explosive devices (VBIEDs) have become the weapon of choice for insurgents in Iraq. At the same time, these devices are becoming increasingly sophisticated and effective. VBIEDs can be difficult to detect during visual inspection of vehicles. This is especially true when explosives have been hidden behind a vehicle"s panels, inside seat cushions, under floorboards, or behind cargo. Even though the explosive may not be visible, vapors of explosive emanating from the device are often present in the vehicle, but the current generation of trace detection equipment has not been sensitive enough to detect these low concentrations of vapor. This paper presents initial test results using the Nomadics Fido sensor for detection of VBIEDs. The sensor is a small, explosives detector with unprecedented levels of sensitivity for detection of nitroaromatic explosives. Fido utilizes fluorescence quenching of novel polymer materials to detect traces of explosive vapor emanating from targets containing explosives. These materials, developed by collaborators at the Massachusetts Institute of Technology (MIT), amplify the quenching response that occurs when molecules of explosive bind to films of the polymer. These materials have enabled development of sensors with performance approaching that of canines trained to detect explosives. The ability of the sensor to detect explosives in vehicles and on persons who have recently been in close proximity to explosives has recently been demonstrated. In these tests, simulated targets were quickly and easily detected using a Fido sensor in conjunction with both direct vapor and swipe sampling methods. The results of these tests suggest that chemical vapor sensing has utility as a means of screening vehicles for explosives at checkpoints and on patrols.

  16. Total reflection X-ray fluorescence as a convenient tool for determination of trace elements in microscale gasoline and diesel

    NASA Astrophysics Data System (ADS)

    Zhang, Airui; Jin, Axiang; Wang, Hai; Wang, Xiaokang; Zha, Pengfei; Wang, Meiling; Song, Xiaoping; Gao, Sitian

    2018-03-01

    Quantitative determination of trace elements like S, Fe, Cu, Mn and Pb in gasoline and S in diesel is of great importance due to the growing concerns over air pollution, human health and engine failure caused by utilization of gasoline and diesel with these harmful elements. A method of total reflection X-ray fluorescence (TXRF) was developed to measure these harmful trace elements in gasoline and diesel. A variety of factors to affect measurement results, including TXRF parameters, microwave-assisted digestion conditions and internal standard element and its addition, were examined to optimize these experimental procedures. The hydrophobic treatment of the surface of quartz reflectors to support the analyte with neutral silicone solutions could prepare thin films of gasoline and diesel digestion solutions for subsequent TXRF analysis. The proposed method shows good potential and reliability to determine the content of harmful trace elements in gasoline and diesel with high sensitivity and accuracy without drawing different standard calibration curves, and can be easily employed to screen gasoline and diesel in routine quality control and assurance.

  17. Determination of trace aluminum by fluorescence quenching method based on catalysis of potassium chlorate oxidizing alizarin red

    NASA Astrophysics Data System (ADS)

    Shao-Qin, Lin; Xuan, Lin; Shi-Rong, Hu; Li-Qing, Zeng; Yan, Wang; Li, Chen; Jia-Ming, Liu; Long-Di, Li

    2005-11-01

    A new method for the determination of trace aluminum has been proposed. It is based on the fact that alizarin red can emit strong and stable fluorescence at 80 °C for 30 min and Al 3+ can effectively catalyze potassium chlorate oxidizing alizarin red to form non-fluorescence complex which cause the fluorescence quenching. The linear dynamic range of this method is 0.040-4.00 ng l -1 with a detection limit of 5.3 pg l -1. The regression equation can be expressed as Δ If = 8.731 + 21.73 c (ng l -1), with the correlation coefficient r = 0.9992 ( n = 6). This sensitive, rapid and accurate method has been applied to the determination of trace aluminum(III) in human hair and tea samples successfully. What is more, the mechanism of catalyzing potassium chlorate oxidizing alizarin red by the fluorescence quenching method is also discussed.

  18. Determination of trace aluminum by fluorescence quenching method based on catalysis of potassium chlorate oxidizing alizarin red.

    PubMed

    Shao-Qin, Lin; Xuan, Lin; Shi-Rong, Hu; Li-Qing, Zeng; Yan, Wang; Li, Chen; Jia-Ming, Liu; Long-Di, Li

    2005-11-01

    A new method for the determination of trace aluminum has been proposed. It is based on the fact that alizarin red can emit strong and stable fluorescence at 80 degrees C for 30 min and Al(3+) can effectively catalyze potassium chlorate oxidizing alizarin red to form non-fluorescence complex which cause the fluorescence quenching. The linear dynamic range of this method is 0.040-4.00 ngl(-1) with a detection limit of 5.3 pgl(-1). The regression equation can be expressed as DeltaI(f)=8.731+21.73c(Al(3+)) (ngl(-1)), with the correlation coefficient r=0.9992 (n=6). This sensitive, rapid and accurate method has been applied to the determination of trace aluminum(III) in human hair and tea samples successfully. What is more, the mechanism of catalyzing potassium chlorate oxidizing alizarin red by the fluorescence quenching method is also discussed.

  19. Texture one zero Dirac neutrino mass matrix with vanishing determinant or trace condition

    NASA Astrophysics Data System (ADS)

    Singh, Madan

    2018-06-01

    In the light of non-zero and relatively large value of rector mixing angle (θ13), we have performed a detailed analysis of texture one zero neutrino mass matrix Mν in the scenario of vanishing determinant/trace conditions, assuming the Dirac nature of neutrinos. In both the scenarios, normal mass ordering is ruled out for all the six possibilities of Mν, however for inverted mass ordering, only two are found to be viable with the current neutrino oscillation data at 3σ confidence level. Numerical and some approximate analytical results are presented.

  20. Simultaneous determination of mushroom toxins α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry.

    PubMed

    Tomková, Jana; Ondra, Peter; Válka, Ivo

    2015-06-01

    This paper presents a method for the simultaneous determination of α-amanitin, β-amanitin and muscarine in human urine by solid-phase extraction (SPE) and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. The method can be used for a diagnostics of mushroom poisonings. Different SPE cartridges were tested for sample preparation, namely hydrophilic modified reversed-phase (Oasis HLB) and polymeric weak cation phase (Strata X-CW). The latter gave better results and therefore it was chosen for the subsequent method optimization and partial validation. In the course of validation, limits of detection, linearity, intraday and interday precisions and recoveries were evaluated. The obtained LOD values of α-amanitin and β-amanitin were 1ng/mL and of muscarine 0.09ng/mL. The intraday and interday precisions of human urine spiked with α-amanitin (10ng/mL), β-amanitin (10ng/mL) and muscarine (1ng/mL) ranged from 6% to 10% and from 7% to 13%, respectively. The developed method was proved to be a relevant tool for the simultaneous determination of the studied mushroom toxins in human urine after mushroom poisoning. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

  1. Biomonitor of Environmental Stress: Coral Trace Metal Analysis

    NASA Astrophysics Data System (ADS)

    Grumet, N.; Hughen, K.

    2006-12-01

    Tropical reef corals are extremely sensitive to changes in environmental conditions and, as a result of environmental degradation and global climate change, coral reefs around the globe are severely threatened. Increased human population and development in tropical regions is leading to higher turbidity and silt loading from terrestrial runoff, increased pesticides and nutrients from agricultural land-use and sewage, and the release of toxic trace metals to coastal waters from industrial pollution. The uptake of these metals and nutrients within the coral skeletal aragonite is a sensitive biomonitor of environmental stresses on coral health. We analyzed 18 trace metals from the surface of coral skeletons collected in Bermuda, Indonesia and Belize to assess a range of threats to coral reef health - including climate change, agricultural runoff and pesticides, and coastal development and tourism. This surface sample network also includes samples representing 4 different coral species. Trace metal analysis was performed on an inductively coupled plasma mass spectrometer (ICP-MS) to a high degree of accuracy and precision at extremely low (ppb) concentrations using a protocol we developed for samples less than 2 mg. Proper cleaning techniques were employed to minimize blank level concentrations for ultra-trace metal ICP-MS solution analysis. However, Zn/Ca and Ni/Ca concentrations remain below analytical detection limits. Initial results indicate that sea surface temperature proxies (e.g., Sr/Ca, B/Ca and Mg/Ca) display similar ratios between the different sites, whereas those metals associated with anthropogenic activities, such as Co, Pb and Cu, are site-specific and are linked to individual environmental stressors. Results from this study will be applied to down core trace metal records in the future. In doing so, we aim to understand the impacts of compounding environmental stresses on coral health, and to identify regional threshold values beyond which corals

  2. General fusion approaches for the age determination of latent fingerprint traces: results for 2D and 3D binary pixel feature fusion

    NASA Astrophysics Data System (ADS)

    Merkel, Ronny; Gruhn, Stefan; Dittmann, Jana; Vielhauer, Claus; Bräutigam, Anja

    2012-03-01

    Determining the age of latent fingerprint traces found at crime scenes is an unresolved research issue since decades. Solving this issue could provide criminal investigators with the specific time a fingerprint trace was left on a surface, and therefore would enable them to link potential suspects to the time a crime took place as well as to reconstruct the sequence of events or eliminate irrelevant fingerprints to ensure privacy constraints. Transferring imaging techniques from different application areas, such as 3D image acquisition, surface measurement and chemical analysis to the domain of lifting latent biometric fingerprint traces is an upcoming trend in forensics. Such non-destructive sensor devices might help to solve the challenge of determining the age of a latent fingerprint trace, since it provides the opportunity to create time series and process them using pattern recognition techniques and statistical methods on digitized 2D, 3D and chemical data, rather than classical, contact-based capturing techniques, which alter the fingerprint trace and therefore make continuous scans impossible. In prior work, we have suggested to use a feature called binary pixel, which is a novel approach in the working field of fingerprint age determination. The feature uses a Chromatic White Light (CWL) image sensor to continuously scan a fingerprint trace over time and retrieves a characteristic logarithmic aging tendency for 2D-intensity as well as 3D-topographic images from the sensor. In this paper, we propose to combine such two characteristic aging features with other 2D and 3D features from the domains of surface measurement, microscopy, photography and spectroscopy, to achieve an increase in accuracy and reliability of a potential future age determination scheme. Discussing the feasibility of such variety of sensor devices and possible aging features, we propose a general fusion approach, which might combine promising features to a joint age determination scheme

  3. [Rapid determination of trace iodate using monolithic column ion-pair chromatography coupled with direct conductivity detection].

    PubMed

    Liu, Yuzhen; Yu, Hong; Li, Siwen

    2011-10-01

    A method was developed on a monolithic column for the fast determination of trace iodate (IO(3)- ) by ion-pair chromatography with direct conductivity detection. The analytes were separated using a mobile phase of tetrabutylammonium hydroxide (TBA)-phthalic acid-acetonitrile on a reversed-phase silica-based monolithic column. The effects of eluent, flow rate and column temperature on the retention of iodate were investigated. The optimized chromatographic conditions for the determination of the anion were as follows: 0. 25 mmol/L TBA-0. 18 mmol/L phthalic acid-3% acetonitrile (pH 5.5) as mobile phase, a flow rate of 4.0 mL/min and a column temperature of 30 degrees C. Under the optimal conditions, retention time of iodate was less than 0. 5 min and the baseline separation of iodate was achieved without any interference by other anions (Cl-, NO , SO4(2)-, I- ). The detection limit (S/N= 3) was 0.36 mg/L for IO(3)- . Relative standard deviation (RSD, n = 5) of chromatographic peak area and retention time were 0. 35% and 0. 28%, respectively. The proposed method was applied to the determination of trace iodate in iodized medicine. The spiked recovery of iodate was 96. 4%. The method is rapid, simple, accurate, reliable, and practical.

  4. Electrochemical Sample Matrix Elimination for Trace Level Potentiometric Detection with Polymeric Membrane Ion-Selective Electrodes

    PubMed Central

    Chumbimuni-Torres, Karin Y.; Calvo-Marzal, Percy; Wang, Joseph; Bakker, Eric

    2008-01-01

    Potentiometric sensors are today sufficiently well understood and optimized to reach ultra-trace level (sub-nanomolar) detection limits for numerous ions. In many cases of practical relevance, however, a high electrolyte background hampers the attainable detection limits. A particularly difficult sample matrix for potentiometric detection is seawater, where the high saline concentration forms a major interfering background and reduces the activity of most trace metals by complexation. This paper describes for the first time a hyphenated system for the online electrochemically modulated preconcentration and matrix elimination (EMPM) of trace metals, combined with a downstream potentiometric detection with solid contact polymeric membrane ion-selective microelectrodes. Following the preconcentration at the bismuth coated electrodes, the deposited metals are oxidized and released to a medium favorable to potentiometric detection, in this case calcium nitrate. Matrix interferences arising from the saline sample medium are thus circumvented. This concept is successfully evaluated with cadmium as a model trace element and offers potentiometric detection down to low parts per billion levels in samples containing 0.5 M NaCl background electrolyte. PMID:18570385

  5. [Determination of eight trace elements in the Swertia davidii Franch by flame atomic absorption spectrometry].

    PubMed

    Li, Tao; Wang, Yuan-zhong; Yu, Hon; Cao, Yu-juan; Zhang, Jing-jing; Liu, Qin

    2007-12-01

    The effects of different sample digestives on the determination of Swertia davidii Franch are compared. Eight trace elements in the Swertia davidii Franch were determined by flame atomic absorption spectrometry. The result shows that the RSD and recovery are better if the Swertia davidii Franch was digested with HNO3-HClO4 (5 : 1) mixed acid. The experimental results show that the detection limits were all smaller than 0.097 microg x mL(-1), the RSDs (n=8) all smaller than 2.34%, and the addition standard recovery (ASR) (n=8) was 89.32%-106.65% for all the elements.

  6. Simultaneous determination of phenolic compounds in Equisetum palustre L. by ultra high performance liquid chromatography with tandem mass spectrometry combined with matrix solid-phase dispersion extraction.

    PubMed

    Wei, Zuofu; Pan, Youzhi; Li, Lu; Huang, Yuyang; Qi, Xiaolin; Luo, Meng; Zu, Yuangang; Fu, Yujie

    2014-11-01

    A method based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with tandem mass spectrometry is presented for the extraction and determination of phenolic compounds in Equisetum palustre. This method combines the high efficiency of matrix solid-phase dispersion extraction and the rapidity, sensitivity, and accuracy of ultra high performance liquid chromatography with tandem mass spectrometry. The influential parameters of the matrix solid-phase dispersion extraction were investigated and optimized. The optimized conditions were as follows: silica gel was selected as dispersing sorbent, the ratio of silica gel to sample was selected to be 2:1 (400/200 mg), and 8 mL of 80% methanol was used as elution solvent. Furthermore, a fast and sensitive ultra high performance liquid chromatography with tandem mass spectrometry method was developed for the determination of nine phenolic compounds in E. palustre. This method was carried out within <6 min, and exhibited satisfactory linearity, precision, and recovery. Compared with ultrasound-assisted extraction, the proposed matrix solid-phase dispersion procedure possessed higher extraction efficiency, and was more convenient and time saving with reduced requirements on sample and solvent amounts. All these results suggest that the developed method represents an excellent alternative for the extraction and determination of active components in plant matrices. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Ultra short laser pulse modification of wave guides

    NASA Astrophysics Data System (ADS)

    Rosenfeld, Arkadi; Ashkenasi, David

    2003-11-01

    The high peak powers of ultra short (ps and sub-ps) pulsed lasers available at relatively low single pulse energies potentially allow for a precise localization of photon energy, either on the surface or inside (transparent) materials. Three dimensional micro structuring of bulk transparent media without any sign of mechanical cracking has shown the potential of ultra short laser processing. In this study, the micro structuring of bulk transparent media was used to modify fused silica and especially the cladding-core interface in normal fused silica wave guides. The idea behind this technique is to enforce a local mismatch for total reflection at the interface at minimal mechanic stress to overcome the barrier for enhanced optical out-coupling. The laser-induced modifications were studied in dependence of pulse width, focal alignment, single pulse energy and pulse overlap. Micro traces with a thickness between 3 and 8 μm were generated with a spacing of 10 μm in the subsurface region using sub-ps and ps laser pulses at a wavelength of 800 nm. The optical leakage enforced by a micro spiral pattern is significant and can be utilized for medical applications or potentially also for telecommunications and fiber laser technology.

  8. Trace elements and common ions in southeastern Idaho snow: Regional air pollutant tracers for source area emissions

    USGS Publications Warehouse

    Abbott, M.; Einerson, J.; Schuster, P.; Susong, D.; Taylor, Howard E.; ,

    2004-01-01

    Snow sampling and analysis methods which produce accurate and ultra-low measurements of trace elements and common ion concentration in southeastern Idaho snow, were developed. Snow samples were collected over two winters to assess trace elements and common ion concentrations in air pollutant fallout across the southeastern Idaho. The area apportionment of apportionment of fallout concentrations measured at downwind location were investigated using pattern recognition and multivariate statistical technical techniques. Results show a high level of contribution from phosphates processing facilities located outside Pocatello in the southern portion of the Eastern Snake River Plain, and no obvious source area profiles other than at Pocatello.

  9. Integrated luminometer for the determination of trace metals in seawater using fluorescence, phosphorescence and chemiluminescence detection

    PubMed Central

    Achterberg, E. P.; Bowie, A. R.; Cannizzaro, V.; Charles, S.; Costa, J. M.; Dubois, F.; Pereiro, R.; San Vicente, B.; Sanz-Medel, A.; Vandeloise, R.; Donckt, E. Vander; Wollast, P.; Yunus, S.

    2002-01-01

    The paper describes an integrated luminometer able to perform fluorescence (FL), room temperature phosphorescence (RTP) and chemiluminescence (CL) measurements on seawater samples. The technical details of the instrumentation are presented together with flow injection (FI) manifolds for the determination of cadmium and zinc (by FL), lead (RTP) and cobalt (CL). The analytical figures of merit are given for each manifold and results are presented for the determination of the four trace metals in seawater reference materials (NASS-5, SLEW-2) and Scheldt estuarine water samples. PMID:18924742

  10. Trace Element Determination and Cardioprotection of Terminalia pallida Fruit Ethanolic Extract in Isoproterenol Induced Myocardial Infarcted Rats by ICP-MS.

    PubMed

    Althaf Hussain, Shaik; Kareem, Mohammed Abdul; Rasool, Shaik Nayab; Al Omar, Suliman Yousef; Saleh, Alwasel; Al-Fwuaires, Manal Abdulrahman; Daddam, Jayasimha Rayalu; Devi, Kodidhela Lakshmi

    2018-01-01

    The trace elements and minerals in Terminalia pallida fruit ethanolic extract (TpFE) were determined by the instrument inductively coupled plasma-mass spectrometry (ICP-MS), and the cardioprotection of TpFE against isoproterenol (ISO)-administered rats was studied. Rats were pretreated with TpFE (100, 300, and 500 mg/kg bw) for 30 days, with concurrent administration of ISO (85 mg/kg bw) for two consecutive days. The levels of trace elements and minerals in TpFE were below the permitted limits of World Health Organization standards. ISO administration significantly increased the heart weight and cardiac marker enzymes in serum, xanthine oxidase, sodium, and calcium in the heart, whereas significantly decreased body weight, reduced glutathione, glutathione-S-transferase, superoxide dismutase, and potassium in the heart. Oral pretreatment of TpFE significantly prevented the ISO-induced alterations. This is the first report that revealed the determination of trace elements and mineral nutrients of TpFE by ICP-MS which plays a principal role in the herbal drug discovery for the treatment of cardiovascular diseases.

  11. Derivatization in gas chromatographic determination of phenol and aniline traces in aqueous media

    NASA Astrophysics Data System (ADS)

    Gruzdev, I. V.; Zenkevich, I. G.; Kondratenok, B. M.

    2015-06-01

    Substituted anilines and phenols are the most common hydrophilic organic environmental toxicants. The principles of gas chromatographic determination of trace amounts of these compounds in aqueous media at concentrations <=0.1 μg litre-1 based on synthesis of their derivatives (derivatization) directly in the aqueous phase are considered. Conversion of relatively hydrophilic analytes into more hydrophobic derivatives makes it possible to achieve such low detection limits and optimize the protocols of extractive preconcentration and selective chromatographic detection. Among the known reactions, this condition is best met by electrophilic halogenation of compounds at the aromatic moiety. The bibliography includes 177 references.

  12. The Determination of Trace Metals in Saline Waters and Biological Tissues Using the Heated Graphite Atomizer

    NASA Technical Reports Server (NTRS)

    Segar, D. A.

    1971-01-01

    A selective, volatalization technique utilizing the heated graphite atomizer atomic absorption technique has been developed for the analysis of iron in sea water. A similar technique may be used to determine vanadium, copper, nickel and cobalt in saline waters when their concentrations are higher than those normally encountered'in unpolluted sea waters. A preliminary solvent extraction using ammonium pyrolidine dithiocarbamate and methyl iso-butyl ketone permits the determination of a number of elements including iron, copper, zinc, nickel, cobalt and lead in sea water. The heated graphite atomized technique has also been applied to the determination of a range of trace transition elements in marine plant and animal tissues.

  13. Official Methods for the Determination of Minerals and Trace Elements in Infant Formula and Milk Products: A Review.

    PubMed

    Poitevin, Eric

    2016-01-01

    The minerals and trace elements that account for about 4% of total human body mass serve as materials and regulators in numerous biological activities in body structure building. Infant formula and milk products are important sources of endogenic and added minerals and trace elements and hence, must comply with regulatory as well as nutritional and safety requirements. In addition, reliable analytical data are necessary to support product content and innovation, health claims, or declaration and specific safety issues. Adequate analytical platforms and methods must be implemented to demonstrate both the compliance and safety assessment of all declared and regulated minerals and trace elements, especially trace-element contaminant surveillance. The first part of this paper presents general information on the mineral composition of infant formula and milk products and their regulatory status. In the second part, a survey describes the main techniques and related current official methods determining minerals and trace elements in infant formula and milk products applied for by various international organizations (AOAC INTERNATIONAL, the International Organization for Standardization, the International Dairy Federation, and the European Committe for Standardization). The third part summarizes method officialization activities by Stakeholder Panels on Infant Formula and Adult Nutritionals and Stakeholder Panel on Strategic Food Analytical Methods. The final part covers a general discussion focusing on analytical gaps and future trends in inorganic analysis that have been applied for in infant formula and milk-based products.

  14. Highly sensitive spectrofluorimetric determination of trace amounts NADP using Europium ion-doxycycline complex probe

    NASA Astrophysics Data System (ADS)

    Peng, Qian; Hou, Faju; Jiang, Chongqiu

    2006-09-01

    A new spectrofluorimetric method was developed for determination of trace amount of Coenzyme II (NADP). Using europium ion-doxycycline (DC) as a fluorescent probe, in the buffer solution of pH 8.44, NADP can remarkably enhance the fluorescence intensity of the Eu 3+-DC complex at λ = 612 nm and the enhanced fluorescence intensity is in proportion to the concentration of NADP. Optimum conditions for the determination of NADP were also investigated. The dynamic range for the determination of NADP is 3.3 × 10 -7 to 6.1 × 10 -6 mol l -1 with detection limit of 6.8 × 10 -8 mol l -1. This method is simple, practical and relatively free interference from coexisting substances and can be successfully applied to determination of NADP in synthetic water samples and in serum samples. Moreover, the enhancement mechanisms of the fluorescence intensity in the Eu 3+-DC system and the Eu 3+-DC-NADP system have been also discussed.

  15. Determination of trace metals and analysis of arsenic species in tropical marine fishes from Spratly islands.

    PubMed

    Li, Jingxi; Sun, Chengjun; Zheng, Li; Jiang, Fenghua; Wang, Shuai; Zhuang, Zhixia; Wang, Xiaoru

    2017-09-15

    Trace metal contents in 38 species of tropical marine fishes harvested from the Spratly islands of China were determined by microwave digestion and inductively coupled plasma mass spectrometry analysis. Arsenic species were determined by high-performance liquid chromatography and inductively coupled plasma mass spectrometry analysis. The average levels of Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Pb, and U in the fish samples were 1.683, 0.350, 0.367, 2.954, 36.615, 0.087, 0.319, 1.566, 21.946, 20.845, 2.526, 3.583, 0.225, 0.140, and 0.061mg·kg -1 , respectively; Fe, Zn, and As were found at high concentrations. The trace metals exhibited significant positive correlation between each other, with r value of 0.610-0.852. Further analysis indicated that AsB (8.560-31.020mg·kg -1 ) was the dominant arsenic species in the fish samples and accounted for 31.48% to 47.24% of the total arsenic. As(III) and As(V) were detected at low concentrations, indicating minimal arsenic toxicity. Copyright © 2017. Published by Elsevier Ltd.

  16. Low-cost ultra-thin broadband terahertz beam-splitter.

    PubMed

    Ung, Benjamin S-Y; Fumeaux, Christophe; Lin, Hungyen; Fischer, Bernd M; Ng, Brian W-H; Abbott, Derek

    2012-02-27

    A low-cost terahertz beam-splitter is fabricated using ultra-thin LDPE plastic sheeting coated with a conducting silver layer. The beam splitting ratio is determined as a function of the thickness of the silver layer--thus any required splitting ratio can be printed on demand with a suitable rapid prototyping technology. The low-cost aspect is a consequence of the fact that ultra-thin LDPE sheeting is readily obtainable, known more commonly as domestic plastic wrap or cling wrap. The proposed beam-splitter has numerous advantages over float zone silicon wafers commonly used within the terahertz frequency range. These advantages include low-cost, ease of handling, ultra-thin thickness, and any required beam splitting ratio can be readily fabricated. Furthermore, as the beam-splitter is ultra-thin, it presents low loss and does not suffer from Fabry-Pérot effects. Measurements performed on manufactured prototypes with different splitting ratios demonstrate a good agreement with our theoretical model in both P and S polarizations, exhibiting nearly frequency-independent splitting ratios in the terahertz frequency range.

  17. Experiment to Characterize Aircraft Volatile Aerosol and Trace-Species Emissions (EXCAVATE)

    NASA Technical Reports Server (NTRS)

    Anderson, B. E.; Branham, H.-S.; Hudgins, C. H.; Plant, J. V.; Ballenthin, J. O.; Miller, T. M.; Viggiano, A. A.; Blake, D. R.; Boudries, H.; Canagaratna, M.

    2005-01-01

    The Experiment to Characterize Aircraft Volatile and Trace Species Emissions (EXCAVATE) was conducted at Langley Research Center (LaRC) in January 2002 and focused upon assaying the production of aerosols and aerosol precursors by a modern commercial aircraft, the Langley B757, during ground-based operation. Remaining uncertainty in the postcombustion fate of jet fuel sulfur contaminants, the need for data to test new theories of particle formation and growth within engine exhaust plumes, and the need for observations to develop air quality models for predicting pollution levels in airport terminal areas were the primary factors motivating the experiment. NASA's Atmospheric Effects of Aviation Project (AEAP) and the Ultra Effect Engine Technology (UEET) Program sponsored the experiment which had the specific objectives of determining ion densities; the fraction of fuel S converted from S(IV) to S(VI); the concentration and speciation of volatile aerosols and black carbon; and gas-phase concentrations of long-chain hydrocarbon and PAH species, all as functions of engine power, fuel composition, and plume age.

  18. Determination of Trace and Volatile Element Abundance Systematics of Lunar Pyroclastic Glasses 74220 and 15426 Using LA-ICP-MS

    NASA Technical Reports Server (NTRS)

    McIntosh, E. Carrie; Porrachia, Magali; McCubbin, Francis M.; Day, James M. D.

    2017-01-01

    Since their recognition as pyroclastic glasses generated by volcanic fire fountaining on the Moon, 74220 and 15426 have garnered significant scientific interest. Early studies recognized that the glasses were particularly enriched in volatile elements on their surfaces. More recently, detailed analyses of the interiors of the glasses, as well as of melt inclusions within olivine grains associated with the 74220 glass beads, have determined high H2O, F, Cl and S contents. Such elevated volatile contents seem at odds with evidence from moderately volatile elements (MVE), such as Zn and K, for a volatile- depleted Moon. In this study, we present initial results from an analytical campaign to study trace element abundances within the pyroclastic glass beads. We report trace element data determined by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for 15426 and 74220.

  19. Determination of trace elements in epiphytic lichens from Bandar Baru Bangi, Selangor using INAA method

    NASA Astrophysics Data System (ADS)

    Khairudin, Nurshafiq Ezam; Siong, Khoo Kok; Siong, Wee Boon

    2014-02-01

    Lichens have been used as effective biomonitors of atmospheric pollutants as they can take up nutrients and pollutants directly from the atmosphere. In this study, trace element contents in epiphytic lichens were determined using INAA method. Samples were collected from 7 sampling locations around Bandar Baru Bangi, Selangor. The elements detected were As (1.73+0.85 mg/kg), Ce (3.65+1.91 mg/kg), Co (0.29+0.12 mg/kg), Cr (5.92+3.54 mg/kg), Cs (0.92+0.25 mg/kg), Eu (0.03+0.02 mg/kg), Fe (1280+760 mg/kg), Hf (0.37+0.18 mg/kg), La (1.52+0.89 mg/kg), Rb (27.7+4.8 mg/kg), Sc (0.33+0.19 mg/kg), Sm (0.28+0.16 mg/kg), Th (1.21+0.62 mg/kg) and Zn (116+27 mg/kg). Comparisons were then made between the elemental concentrations obtained and the baseline data from literature. Results showed that most of the elements were within the concentration range of the baseline data. Enrichment factors (EF) of the trace element in lichens showed that most of the elements were within the range of the baseline data except for As which was found to be slightly enriched (EF: 13.2 - 28.5). Regression analysis indicated significant correlation (p<0.05) with Sc for most of the elements which signifies crustal input except for Cs and Rb. The poor correlations of Cs and Rb with Sc may be due to the mobility of these elements. In summary, trace element data obtained using INAA were very useful and demonstrated that lichens were suitable biomonitors for identifying potential trace element pollutants in ambient air around the sampling area.

  20. Ultra-widefield retinal imaging through a black intraocular lens.

    PubMed

    Yusuf, Imran H; Fung, Timothy H M; Patel, Chetan K

    2015-09-01

    To evaluate the feasibility of ultra-widefield retinal imaging in patients with near infrared (IR)-transmitting black intraocular lenses (IOLs). Oxford Eye Hospital, Oxford, United Kingdom. Laboratory evaluation of a diagnostic technology with interventional case report. The field of retinal imaging through a Morcher poly(methyl methacrylate) (PMMA) black IOL was determined in a purpose-built adult schematic model eye with the HRA2 Spectralis confocal scanning laser ophthalmoscope using standard imaging, Staurenghi retina lens-assisted imaging, and ultra-widefield noncontact imaging. Retinal imaging using each modality was then performed on a patient implanted with another Morcher PMMA black IOL model. Ultra-widefield noncontact imaging and lens-assisted imaging captured up to 150 degrees of field (versus 40 degrees with a standard confocal scanning laser ophthalmoscope). Ultra-widefield retinal images were successfully acquired in a patient eye with a black IOL. This study has identified the first ultra-widefield retinal imaging modalities for patients with near IR-transmitting black IOLs. Should larger studies confirm this finding, noncontact ultra-widefield confocal scanning laser ophthalmoscopy might be considered the gold standard imaging technique for retinal surveillance in patients with near IR-transmitting black IOLs. No author has a financial or proprietary interest in any material or method mentioned. Copyright © 2015 ASCRS and ESCRS. Published by Elsevier Inc. All rights reserved.

  1. Determination of selected trace elements in foodstuffs and biological materials by destructive neutron activation analysis.

    PubMed

    Bayat, I; Etehadiyan, M; Ansar, M

    1995-01-01

    Concentration of trace elements in Nescafé, Fariman sugar, and Sadaf turmeric and mercury content in cancerous blood were determined by radiochemical, neutron activation analysis. By this separation method levels of 110mAg, 198Au, 203Hg, 76Se, 51Cr, 24Na, 42K, 99Mo, 122Sb, 82Br, 59Fe, 60Co were measured without interference in the gamma spectroscopy. A nondestructive method has also been used for the analysis of sodium, potassium, and bromine.

  2. Neurient: An Algorithm for Automatic Tracing of Confluent Neuronal Images to Determine Alignment

    PubMed Central

    Mitchel, J.A.; Martin, I.S.

    2013-01-01

    A goal of neural tissue engineering is the development and evaluation of materials that guide neuronal growth and alignment. However, the methods available to quantitatively evaluate the response of neurons to guidance materials are limited and/or expensive, and may require manual tracing to be performed by the researcher. We have developed an open source, automated Matlab-based algorithm, building on previously published methods, to trace and quantify alignment of fluorescent images of neurons in culture. The algorithm is divided into three phases, including computation of a lookup table which contains directional information for each image, location of a set of seed points which may lie along neurite centerlines, and tracing neurites starting with each seed point and indexing into the lookup table. This method was used to obtain quantitative alignment data for complex images of densely cultured neurons. Complete automation of tracing allows for unsupervised processing of large numbers of images. Following image processing with our algorithm, available metrics to quantify neurite alignment include angular histograms, percent of neurite segments in a given direction, and mean neurite angle. The alignment information obtained from traced images can be used to compare the response of neurons to a range of conditions. This tracing algorithm is freely available to the scientific community under the name Neurient, and its implementation in Matlab allows a wide range of researchers to use a standardized, open source method to quantitatively evaluate the alignment of dense neuronal cultures. PMID:23384629

  3. Alkaline and ultrasonic dissolution of biological materials for trace silicon determination

    PubMed Central

    Viveros, Robert D.; Liberman, Alexander; Trogler, William C.; Kummel, Andrew C.

    2015-01-01

    A simple method for trace elemental determination in biological tissue has been developed. Novel nanomaterials with biomedical applications necessitate the determination of the in vivo fate of the materials to understand their toxicological profile. Hollow iron-doped calcined silica nanoshells have been used as a model to demonstrate that potassium hydroxide and bath sonication at 50 °C can extract elements from alkaline-soluble nanomaterials. After alkali digestion, nitric acid is used to adjust the pH into a suitable range for analysis using techniques such as inductively coupled plasma optical emission spectrometry which require neutral or acidic analytes. In chicken liver phantoms injected with the nanoshells, 96% of the expected silicon concentration was detected. This value was in good agreement with the 94% detection efficiency of nanoshells dissolved in aqueous solution as a control for potential sample matrix interference. Nanoshell detection was further confirmed in a mouse 24 h after intravenous administration; the measured silica above baseline was 35 times greater or more than the standard deviations of the measurements. This method provides a simple and accurate means to quantify alkaline-soluble nanomaterials in biological tissue. PMID:25909037

  4. Ion Imprinted Polymer for Preconcentration and Determination of Ultra-Trace Cadmium, Employing Flow Injection Analysis with Thermo Spray Flame Furnace Atomic Absorption Spectrometry.

    PubMed

    do Lago, Ayla Campos; Marchioni, Camila; Mendes, Tássia Venga; Wisniewski, Célio; Fadini, Pedro Sergio; Luccas, Pedro Orival

    2016-11-01

    This work proposes a preconcentration method using an ion imprinted polymer (IIP) for determination of cadmium, in several samples, employing a mini-column filled with the polymer coupled into a flow injection analysis system with detection by thermospray flame furnace atomic absorption spectrometry (FIA-TS-FF-AAS). The polymer was synthesized via bulk using methacrylic acid and vinylimidazole as a functional monomer. For the FIA system initial assessment, the variables: pH, eluent concentration and buffer concentration were studied, employing a 23 full factorial design. To obtain the optimum values for each significant variable, a Doehlert matrix was employed. After the optimization conditions as: pH 5.8, eluent (HNO3) concentration of 0.48 mol L -1 and buffer concentration of 0.01 mol L -1 , were adopted. The proposed method showed a linear response in the range of 0.081-10.0 μg L -1 , limits detection and quantification of 0.024 and 0.081 μg L -1 , respectively; preconcentration factor of 165, consumptive index of 0.06 mL, concentration efficiency 132 min -1 , and frequency of readings equal to 26 readings h -1 The accuracy was checked by analysis of certified reference materials for trace metals and recovery tests. The obtained results were in agreement with 95% confidence level (t-test). The method was adequate to apply in samples of: jewelry (earrings) (2.38 ± 0.28 μg kg -1 ), black tea (1.09 ± 0.15 μg kg -1 ), green tea (3.85 ± 0.13 μg kg -1 ), cigarette tobacco (38.27 ± 0.22 μg kg -1 ), and hair (0.35 ± 0.02 μg kg -1 ). © The Author(s) 2016.

  5. Ultra low-level measurements of actinides by sector field ICP-MS.

    PubMed

    Pointurier, F; Baglan, N; Hémet, P

    2004-01-01

    In the present work, a double-focusing sector field inductively coupled plasma-mass spectrometer was optimised for ultra trace and isotopic analyses of actinide long-lived isotopes in low concentration solutions of the fgml(-1) to the ngml(-1) range. Sensitivities of about 3GHz/(microgml(-1)), with as low a background as 0.1cps, were obtained for U using a conventional concentric pneumatic nebuliser. Detection limits are below the fg range for 239Pu and 240Pu. With natural U, a precision lower than 0.5% RSD is currently obtained for 235U/238U isotopic ratio at the 200pgml(-1) level.

  6. Comparison of ultra-widefield fluorescein angiography with the Heidelberg Spectralis® noncontact ultra-widefield module versus the Optos® Optomap®

    PubMed Central

    Witmer, Matthew T; Parlitsis, George; Patel, Sarju; Kiss, Szilárd

    2013-01-01

    Purpose To compare ultra-widefield fluorescein angiography imaging using the Optos® Optomap® and the Heidelberg Spectralis® noncontact ultra-widefield module. Methods Five patients (ten eyes) underwent ultra-widefield fluorescein angiography using the Optos® panoramic P200Tx imaging system and the noncontact ultra-widefield module in the Heidelberg Spectralis® HRA+OCT system. The images were obtained as a single, nonsteered shot centered on the macula. The area of imaged retina was outlined and quantified using Adobe® Photoshop® C5 software. The total area and area within each of four visualized quadrants was calculated and compared between the two imaging modalities. Three masked reviewers also evaluated each quadrant per eye (40 total quadrants) to determine which modality imaged the retinal vasculature most peripherally. Results Optos® imaging captured a total retinal area averaging 151,362 pixels, ranging from 116,998 to 205,833 pixels, while the area captured using the Heidelberg Spectralis® was 101,786 pixels, ranging from 73,424 to 116,319 (P = 0.0002). The average area per individual quadrant imaged by Optos® versus the Heidelberg Spectralis® superiorly was 32,373 vs 32,789 pixels, respectively (P = 0.91), inferiorly was 24,665 vs 26,117 pixels, respectively (P = 0.71), temporally was 47,948 vs 20,645 pixels, respectively (P = 0.0001), and nasally was 46,374 vs 22,234 pixels, respectively (P = 0.0001). The Heidelberg Spectralis® was able to image the superior and inferior retinal vasculature to a more distal point than was the Optos®, in nine of ten eyes (18 of 20 quadrants). The Optos® was able to image the nasal and temporal retinal vasculature to a more distal point than was the Heidelberg Spectralis®, in ten of ten eyes (20 of 20 quadrants). Conclusion The ultra-widefield fluorescein angiography obtained with the Optos® and Heidelberg Spectralis® ultra-widefield imaging systems are both excellent modalities that provide views of the

  7. Comparison of ultra-widefield fluorescein angiography with the Heidelberg Spectralis(®) noncontact ultra-widefield module versus the Optos(®) Optomap(®).

    PubMed

    Witmer, Matthew T; Parlitsis, George; Patel, Sarju; Kiss, Szilárd

    2013-01-01

    To compare ultra-widefield fluorescein angiography imaging using the Optos(®) Optomap(®) and the Heidelberg Spectralis(®) noncontact ultra-widefield module. Five patients (ten eyes) underwent ultra-widefield fluorescein angiography using the Optos(®) panoramic P200Tx imaging system and the noncontact ultra-widefield module in the Heidelberg Spectralis(®) HRA+OCT system. The images were obtained as a single, nonsteered shot centered on the macula. The area of imaged retina was outlined and quantified using Adobe(®) Photoshop(®) C5 software. The total area and area within each of four visualized quadrants was calculated and compared between the two imaging modalities. Three masked reviewers also evaluated each quadrant per eye (40 total quadrants) to determine which modality imaged the retinal vasculature most peripherally. Optos(®) imaging captured a total retinal area averaging 151,362 pixels, ranging from 116,998 to 205,833 pixels, while the area captured using the Heidelberg Spectralis(®) was 101,786 pixels, ranging from 73,424 to 116,319 (P = 0.0002). The average area per individual quadrant imaged by Optos(®) versus the Heidelberg Spectralis(®) superiorly was 32,373 vs 32,789 pixels, respectively (P = 0.91), inferiorly was 24,665 vs 26,117 pixels, respectively (P = 0.71), temporally was 47,948 vs 20,645 pixels, respectively (P = 0.0001), and nasally was 46,374 vs 22,234 pixels, respectively (P = 0.0001). The Heidelberg Spectralis(®) was able to image the superior and inferior retinal vasculature to a more distal point than was the Optos(®), in nine of ten eyes (18 of 20 quadrants). The Optos(®) was able to image the nasal and temporal retinal vasculature to a more distal point than was the Heidelberg Spectralis(®), in ten of ten eyes (20 of 20 quadrants). The ultra-widefield fluorescein angiography obtained with the Optos(®) and Heidelberg Spectralis(®) ultra-widefield imaging systems are both excellent modalities that provide views of the

  8. Determining trace gas flux from container-grown woody ornamentals

    USDA-ARS?s Scientific Manuscript database

    In recent years, anthropogenic climate change and its effects on the global environment has garnered significant attention from the scientific community. Increased trace gas emissions (CO2, CH4, and N2O) are widely believed to be the driving force behind global warming. Agriculture is a large contri...

  9. Using MOF-74 for Hg{sup 2+} removal from ultra-low concentration aqueous solution

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

    Xiong, Yang Yang; Li, Jian Qiang; Gong, Le Le

    Mercury (Hg{sup 2+}) ions have very high toxicity and widely spread as environmental pollutants. At present, many efforts have been taken to remove the hazardous materials of mercury(II) by adsorption, and it is highly desirable to develop a novel adsorbent with high adsorptive capacities. However it is still a big challenge to remove the ultra-low-concentration mercury ions from water. In this paper, MOF-74-Zn is explored for such function, showing high removal rate of Hg(II) from water without any pretreatment, especially for the ultra-trace Hg(II) ions in the ppb magnitude with the removal rate reaching to 54.48%, 69.71%, 72.26% when themore » initial concentration of Hg(II) is 20ppb, 40ppb, 50ppb, respectively. - Graphical abstract: The absorption of mercury ions on MOF-74-Zn is due to somewhat weak interactions between MOF skeleton that is composed of carboxylate and hydroxy group and Hg2+ ions. - Highlights: • MOF-74-Zn shows high removal rate of Hg(II) from water without any pretreatment. • The MOF-74-Zn has a notable performance at ultra-low concentration of Hg(II). • MOF-74-Zn shows the potential for Hg(II) removal from industrial waste water.« less

  10. Designable ultra-smooth ultra-thin solid-electrolyte interphases of three alkali metal anodes.

    PubMed

    Gu, Yu; Wang, Wei-Wei; Li, Yi-Juan; Wu, Qi-Hui; Tang, Shuai; Yan, Jia-Wei; Zheng, Ming-Sen; Wu, De-Yin; Fan, Chun-Hai; Hu, Wei-Qiang; Chen, Zhao-Bin; Fang, Yuan; Zhang, Qing-Hong; Dong, Quan-Feng; Mao, Bing-Wei

    2018-04-09

    Dendrite growth of alkali metal anodes limited their lifetime for charge/discharge cycling. Here, we report near-perfect anodes of lithium, sodium, and potassium metals achieved by electrochemical polishing, which removes microscopic defects and creates ultra-smooth ultra-thin solid-electrolyte interphase layers at metal surfaces for providing a homogeneous environment. Precise characterizations by AFM force probing with corroborative in-depth XPS profile analysis reveal that the ultra-smooth ultra-thin solid-electrolyte interphase can be designed to have alternating inorganic-rich and organic-rich/mixed multi-layered structure, which offers mechanical property of coupled rigidity and elasticity. The polished metal anodes exhibit significantly enhanced cycling stability, specifically the lithium anodes can cycle for over 200 times at a real current density of 2 mA cm -2 with 100% depth of discharge. Our work illustrates that an ultra-smooth ultra-thin solid-electrolyte interphase may be robust enough to suppress dendrite growth and thus serve as an initial layer for further improved protection of alkali metal anodes.

  11. Ultra-low background mass spectrometry for rare-event searches

    NASA Astrophysics Data System (ADS)

    Dobson, J.; Ghag, C.; Manenti, L.

    2018-01-01

    Inductively Coupled Plasma Mass Spectrometry (ICP-MS) allows for rapid, high-sensitivity determination of trace impurities, notably the primordial radioisotopes 238U and 232Th, in candidate materials for low-background rare-event search experiments. We describe the setup and characterisation of a dedicated low-background screening facility at University College London where we operate an Agilent 7900 ICP-MS. The impact of reagent and carrier gas purity is evaluated and we show that twice-distilled ROMIL-SpATM-grade nitric acid and zero-grade Ar gas delivers similar sensitivity to ROMIL-UpATM-grade acid and research-grade gas. A straightforward procedure for sample digestion and analysis of materials with U/Th concentrations down to 10 ppt g/g is presented. This includes the use of 233U and 230Th spikes to correct for signal loss from a range of sources and verification of 238U and 232Th recovery through digestion and analysis of a certified reference material with a complex sample matrix. Finally, we demonstrate assays and present results from two sample preparation and assay methods: a high-sensitivity measurement of ultra-pure Ti using open digestion techniques, and a closed vessel microwave digestion of a nickel-chromium-alloy using a multi-acid mixture.

  12. Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

    PubMed

    Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

    2013-11-15

    A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Improving multi-GNSS ultra-rapid orbit determination for real-time precise point positioning

    NASA Astrophysics Data System (ADS)

    Li, Xingxing; Chen, Xinghan; Ge, Maorong; Schuh, Harald

    2018-03-01

    Currently, with the rapid development of multi-constellation Global Navigation Satellite Systems (GNSS), the real-time positioning and navigation are undergoing dramatic changes with potential for a better performance. To provide more precise and reliable ultra-rapid orbits is critical for multi-GNSS real-time positioning, especially for the three merging constellations Beidou, Galileo and QZSS which are still under construction. In this contribution, we present a five-system precise orbit determination (POD) strategy to fully exploit the GPS + GLONASS + BDS + Galileo + QZSS observations from CDDIS + IGN + BKG archives for the realization of hourly five-constellation ultra-rapid orbit update. After adopting the optimized 2-day POD solution (updated every hour), the predicted orbit accuracy can be obviously improved for all the five satellite systems in comparison to the conventional 1-day POD solution (updated every 3 h). The orbit accuracy for the BDS IGSO satellites can be improved by about 80, 45 and 50% in the radial, cross and along directions, respectively, while the corresponding accuracy improvement for the BDS MEO satellites reaches about 50, 20 and 50% in the three directions, respectively. Furthermore, the multi-GNSS real-time precise point positioning (PPP) ambiguity resolution has been performed by using the improved precise satellite orbits. Numerous results indicate that combined GPS + BDS + GLONASS + Galileo (GCRE) kinematic PPP ambiguity resolution (AR) solutions can achieve the shortest time to first fix (TTFF) and highest positioning accuracy in all coordinate components. With the addition of the BDS, GLONASS and Galileo observations to the GPS-only processing, the GCRE PPP AR solution achieves the shortest average TTFF of 11 min with 7{°} cutoff elevation, while the TTFF of GPS-only, GR, GE and GC PPP AR solution is 28, 15, 20 and 17 min, respectively. As the cutoff elevation increases, the reliability and accuracy of GPS-only PPP AR solutions

  14. WET EFFLUENT PARALLEL PLATE DIFFUSION DENUDER COUPLED CAPILLARY ION CHROMATOGRAPH FOR THE DETERMINATION OF ATMOSPHERIC TRACE GASES. (R825344)

    EPA Science Inventory

    We describe an inexpensive, compact parallel plate diffusion denuder coupled capillary IC system for the determination of soluble ionogenic atmospheric trace gases. The active sampling area (0.6×10 cm) of the denuder is formed in a novel manner by thermally bonding silica ge...

  15. Fast and sensitive analysis of beta blockers by ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry.

    PubMed

    Tomková, Jana; Ondra, Peter; Kocianová, Eva; Václavík, Jan

    2017-07-01

    This paper presents a method for the determination of acebutolol, betaxolol, bisoprolol, metoprolol, nebivolol and sotalol in human serum by liquid-liquid extraction and ultra-high-performance liquid chromatography coupled with ultra-high-resolution TOF mass spectrometry. After liquid-liquid extraction, beta blockers were separated on a reverse-phase analytical column (Acclaim RS 120; 100 × 2.1 mm, 2.2 μm). The total run time was 6 min for each sample. Linearity, limit of detection, limit of quantification, matrix effects, specificity, precision, accuracy, recovery and sample stability were evaluated. The method was successfully applied to the therapeutic drug monitoring of 108 patients with hypertension. This method was also used for determination of beta blockers in 33 intoxicated patients. Copyright © 2016 John Wiley & Sons, Ltd.

  16. Major and minor oxide and trace element determination in silicate rocks by direct current plasma optical emission echelle spectrometry

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

    Bankston, D.C.; Humphris, S.E.; Thompson, G.

    1979-07-01

    A technique for the determination of major concentrations of SiO/sub 2/, Al/sub 2/O/sub 3/, Fe/sub 2/O/sub 3/, MgO, CaO, Na/sub 2/O, and K/sub 2/O, minor levels of TiO/sub 2/, P/sub 2/O/sub 5/, and MnO, and trace concentrations of Ba, Cr, Cu, Ni, Sr, V, and Zn, in semi-microsamples 200 mg) of powdered whole rock, is described. Chemically diverse standard reference rocks are used both for calibration and assessment of accuracy. A lithium metaborate fusion melt of each standard or sample is dissolved in dilute HNO/sub 3/ containing Cs/sup +/ at a level of 0.2% (w/v). The resulting solution is usedmore » to perform all analyses except those for Na/sub 2/O and K/sub 2/O, which are determined in a portion of the original sample solution wherein the Cs/sup +/ concentration has been raised to 0.32% (w/v). Analyses of both portions of each sample solution are performed using an optical emission spectrometer/spectrograph equipped with an echelle monochromator and a dc argon plasma excitation source. Trace element detection limits ranged from 2 ppM for Cu to 15 ppM for Zn. A study of precision based on replicate determinations in three splits of the proposed USGS reference basalt BHVO-1 yielded the following results: (1) For analyses of the major and minor oxide constituents, values of the percent relative standard deviation (RSD) ranged from 1 for CaO, to 21 for P/sub 2/O/sub 5/. 2) For trace element determinations, values of the RSD ranged from 2 for Cu, to 19 for Zn. 2 figures, 11 tables.« less

  17. Accuracy of trace element determinations in alternate fuels

    NASA Technical Reports Server (NTRS)

    Greenbauer-Seng, L. A.

    1980-01-01

    NASA-Lewis Research Center's work on accurate measurement of trace level of metals in various fuels is presented. The differences between laboratories and between analytical techniques especially for concentrations below 10 ppm, are discussed, detailing the Atomic Absorption Spectrometry (AAS) and DC Arc Emission Spectrometry (dc arc) techniques used by NASA-Lewis. Also presented is the design of an Interlaboratory Study which is considering the following factors: laboratory, analytical technique, fuel type, concentration and ashing additive.

  18. STAR FORMATION IN ULTRA-FAINT DWARFS: CONTINUOUS OR SINGLE-AGE BURSTS?

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

    Webster, David; Bland-Hawthorn, Joss; Sutherland, Ralph, E-mail: d.webster@physics.usyd.edu.au

    2015-01-30

    We model the chemical evolution of six ultra-faint dwarfs (UFDs): Bootes I, Canes Venatici II, Coma Berenices, Hercules, Leo IV, and Ursa Major I based on their recently determined star formation histories. We show that two single-age bursts cannot explain the observed [α/Fe] versus [Fe/H] distribution in these galaxies and that some self-enrichment is required within the first burst. An alternative scenario is modeled, in which star formation is continuous except for short interruptions when one or more supernovae temporarily blow the dense gas out from the center of the system. This model allows for self-enrichment and can reproduce themore » chemical abundances of the UFDs in which the second burst is only a trace population. We conclude that the most likely star formation history is one or two extended periods of star formation, with the first burst lasting for at least 100 Myr. As found in earlier work, the observed properties of UFDs can be explained by formation at a low mass (M{sub vir}∼10{sup 7} M{sub ⊙}), rather than being stripped remnants of much larger systems.« less

  19. An Efficient Ray-Tracing Method for Determining Terrain Intercepts in EDL Simulations

    NASA Technical Reports Server (NTRS)

    Shidner, Jeremy D.

    2016-01-01

    The calculation of a ray's intercept from an arbitrary point in space to a prescribed surface is a common task in computer simulations. The arbitrary point often represents an object that is moving according to the simulation, while the prescribed surface is fixed in a defined frame. For detailed simulations, this surface becomes complex, taking the form of real-world objects such as mountains, craters or valleys which require more advanced methods to accurately calculate a ray's intercept location. Incorporation of these complex surfaces has commonly been implemented in graphics systems that utilize highly optimized graphics processing units to analyze such features. This paper proposes a simplified method that does not require computationally intensive graphics solutions, but rather an optimized ray-tracing method for an assumed terrain dataset. This approach was developed for the Mars Science Laboratory mission which landed on the complex terrain of Gale Crater. First, this paper begins with a discussion of the simulation used to implement the model and the applicability of finding surface intercepts with respect to atmosphere modeling, altitude determination, radar modeling, and contact forces influencing vehicle dynamics. Next, the derivation and assumptions of the intercept finding method are presented. Key assumptions are noted making the routines specific to only certain types of surface data sets that are equidistantly spaced in longitude and latitude. The derivation of the method relies on ray-tracing, requiring discussion on the formulation of the ray with respect to the terrain datasets. Further discussion includes techniques for ray initialization in order to optimize the intercept search. Then, the model implementation for various new applications in the simulation are demonstrated. Finally, a validation of the accuracy is presented along with the corresponding data sets used in the validation. A performance summary of the method will be shown using

  20. Gamma-ray spectrometry of ultra low levels of radioactivity within the material screening program for the GERDA experiment.

    PubMed

    Budjás, D; Gangapshev, A M; Gasparro, J; Hampel, W; Heisel, M; Heusser, G; Hult, M; Klimenko, A A; Kuzminov, V V; Laubenstein, M; Maneschg, W; Simgen, H; Smolnikov, A A; Tomei, C; Vasiliev, S I

    2009-05-01

    In present and future experiments in the field of rare events physics a background index of 10(-3) counts/(keV kg a) or better in the region of interest is envisaged. A thorough material screening is mandatory in order to achieve this goal. The results of a systematic study of radioactive trace impurities in selected materials using ultra low-level gamma-ray spectrometry in the framework of the GERDA experiment are reported.

  1. Determining the Environmental Benefits of Ultra High Performance Concrete as a Bridge Construction Material

    NASA Astrophysics Data System (ADS)

    Lande Larsen, Ingrid; Granseth Aasbakken, Ida; O'Born, Reyn; Vertes, Katalin; Terje Thorstensen, Rein

    2017-10-01

    Ultra High Performance Concrete (UHPC) is a material that is attracting attention in the construction industry due to the high mechanical strength and durability, leading to structures having low maintenance requirements. The production of UHPC, however, has generally higher environmental impact than normal strength concrete due to the increased demand of cement required in the concrete mix. What is still not sufficiently investigated, is if the longer lifetime, slimmer construction and lower maintenance requirements lead to a net environmental benefit compared to standard concrete bridge design. This study utilizes life cycle assessment (LCA) to determine the lifetime impacts of two comparable highway crossing footbridges spanning 40 meters, designed respectively with UHPC and normal strength concrete. The results of the study show that UHPC is an effective material for reducing lifetime emissions from construction and maintenance of long lasting infrastructure, as the UHPC design outperforms the normal strength concrete bridge in most impact categories.

  2. Stanford-USGS shrimp-RG ion microprobe: A new approach to determining the distribution of trace elements in coal

    USGS Publications Warehouse

    Kolker, A.; Wooden, J.L.; Persing, H.M.; Zielinski, R.A.

    2000-01-01

    The distribution of Cr and other trace metals of environmental interest in a range of widely used U.S. coals was investigated using the Stanford-USGS SHRIMP-RG ion microprobe . Using the oxygen ion source, concentrations of Cr (11 to 176 ppm), V (23 to 248 ppm), Mn (2 to 149 ppm), Ni (2 to 30 ppm), and 13 other elements were determined in illite/smectite, a group of clay minerals commonly present in coal. The results confirm previous indirect or semi-quantitative determinations indicating illite/smectite to be an important host of these metals. Calibration was achieved using doped aluminosilicate-glass synthetic standards and glasses prepared from USGS rock standards. Grains for analysis were identified optically, and confirmed by 1) precursory electron microprobe analysis and wavelength-dispersive compositional mapping, and 2) SHRIMP-RG major element data obtained concurrently with trace element results. Follow-up investigations will focus on the distribution of As and other elements that are more effectively ionized with the cesium primary beam currently being tested.

  3. Fractionation of trace elements in agricultural soils using ultrasound assisted sequential extraction prior to inductively coupled plasma mass spectrometric determination.

    PubMed

    Matong, Joseph M; Nyaba, Luthando; Nomngongo, Philiswa N

    2016-07-01

    The main objectives of this study were to determine the concentration of fourteen trace elements and to investigate their distribution as well as a contamination levels in selected agricultural soils. An ultrasonic assisted sequential extraction procedure derived from three-step BCR method was used for fractionation of trace elements. The total concentration of trace elements in soil samples was obtained by total digestion method in soil samples with aqua regia. The results of the extractable fractions revealed that most of the target trace elements can be transferred to the human being through the food chain, thus leading to serious human health. Enrichment factor (EF), geo-accumulation index (Igeo), contamination factor (CF), risk assessment code (RAC) and individual contamination factors (ICF) were used to assess the environmental impacts of trace metals in soil samples. The EF revealed that Cd was enriched by 3.1-7.2 (except in Soil 1). The Igeo results showed that the soils in the study area was moderately contaminated with Fe, and heavily to extremely polluted with Cd. The soil samples from the unplanted field was found to have highest contamination factor for Cd and lowest for Pb. Soil 3 showed a high risk for Tl and Cd with RAC values of greater than or equal to 50%. In addition, Fe, Ni, Cu, V, As, Mo (except Soil 2), Sb and Pb posed low environmental risk. The modified BCR sequential extraction method provided more information about mobility and environmental implication of studied trace elements in the study area. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Compliance of Ultra-Orthodox and secular pedestrians with traffic lights in Ultra-Orthodox and secular locations.

    PubMed

    Rosenbloom, Tova; Shahar, Amit; Perlman, Amotz

    2008-11-01

    Following a previous study that revealed the disobedience of Ultra-Orthodox citizens, as compared to secular citizens, of traffic lights at crosswalks, the present study examined the road habits of 995 Ultra-Orthodox and secular pedestrians in neighboring Ultra-Orthodox and secular cities. Using an observation grid designed specially for this study, the pedestrians were observed at two crosswalks--one in an Ultra-Orthodox city and one in a secular city--as far as similar traffic parameters, using a logistic regression. The tendency to cross on a red light was assessed as a function of estimated age, gender, religiosity, location (religious/secular), the duration of the red light, the number of vehicles crossing and the number of pedestrians waiting at the curb. Ultra-Orthodox pedestrians committed more violations than secular pedestrians did, and there were more road violations in the Ultra-Orthodox location than there were in the secular location. Fewer traffic violations were committed by "local" pedestrians (Ultra-Orthodox pedestrians in the Ultra-Orthodox location and secular pedestrians in the secular location) than by "foreigners" (Ultra-Orthodox pedestrians in the secular location and secular pedestrians in the Ultra-Orthodox location). The odds of crossing on a red light decreased as a function of both the number of people waiting at the curb and the number of vehicles. Consistent with previous research, males crossed on red much more than females did, regardless of religiosity and location. Our discussion focuses on theoretical and practical explanations of the findings.

  5. [A technological study on the extraction of ultra-fine powder of Panax notoginsen].

    PubMed

    Huang, Yaohai; Huang, Mingqing; Zeng, Huifang; Guo, Wei; Xi, Ping

    2005-12-01

    To investigate the extraction of ultra-fine powder Panax notoginsen. The extraction rate of ginseng saponin Rg1, Re, Rb1, notoginseng saponin R1 and filtrated time were determined by alcoholic and aqueous extraction of Panax notoginsen in tablet, coarse powder, ultra-fine powder and recostitution granules of ultra-fine powder. The filtered time of ultra-fine powder of Panax notoginsen extraction and that of the tablet of Panax notoginsen extraction were similar, while the extraction rates of various saponins of it were high. The method of aqueous extrction in ltra-fine powder of Panax notoginsen is easy in filtrationer, higher in extraction rate of Panax notoginsen and lower in production cost.

  6. Trace element analysis of rough diamond by LA-ICP-MS: a case of source discrimination?

    PubMed

    Dalpé, Claude; Hudon, Pierre; Ballantyne, David J; Williams, Darrell; Marcotte, Denis

    2010-11-01

    Current profiling of rough diamond source is performed using different physical and/or morphological techniques that require strong knowledge and experience in the field. More recently, chemical impurities have been used to discriminate diamond source and with the advance of laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) empirical profiling of rough diamonds is possible to some extent. In this study, we present a LA-ICP-MS methodology that we developed for analyzing ultra-trace element impurities in rough diamond for origin determination ("profiling"). Diamonds from two sources were analyzed by LA-ICP-MS and were statistically classified by accepted methods. For the two diamond populations analyzed in this study, binomial logistic regression produced a better overall correct classification than linear discriminant analysis. The results suggest that an anticipated matrix match reference material would improve the robustness of our methodology for forensic applications. © 2010 American Academy of Forensic Sciences.

  7. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; preparation procedure for aquatic biological material determined for trace metals

    USGS Publications Warehouse

    Hoffman, Gerald L.

    1996-01-01

    A method for the chemical preparation of tissue samples that are subsequently analyzed for 22 trace metals is described. The tissue-preparation procedure was tested with three National Institute of Standards and Technology biological standard reference materials and two National Water Quality Laboratory homogenized biological materials. A low-temperature (85 degrees Celsius) nitric acid digestion followed by the careful addition of hydrogen peroxide (30-percent solution) is used to decompose the biological material. The solutions are evaporated to incipient dryness, reconstituted with 5 percent nitric acid, and filtered. After filtration the solutions were diluted to a known volume and analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and cold vapor-atomic absorption spectrophotometry (CV-AAS). Many of the metals were determined by both ICP-MS and ICP-AES. This report does not provide a detailed description of the instrumental procedures and conditions used with the three types of instrumentation for the quantitation of trace metals determined in this study. Statistical data regarding recovery, accuracy, and precision for individual trace metals determined in the biological material tested are summarized.

  8. Trace metal determination in natural waters by automated solid phase extraction system and ICP-MS: the influence of low level Mg and Ca.

    PubMed

    Wang, Bo-Shian; Lee, Chih-Ping; Ho, Tung-Yuan

    2014-10-01

    A fully automated high pressure pretreatment system with Nobias Chelate-PA1 resin (PA1) was developed for trace metal determination by ICP-MS in natural waters. By varying the concentrations of Mg and Ca to mimic the concentrations in the eluate obtained by PA1 or iminodiacetate type resins, the overall analytical performance of the system was assessed for the determination of Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Cd, Ag, Pb and REE. Comparing with the low mM level Mg and Ca (both ranging from 1 to 4mM) eluted by iminodiacetate type resins, the eluate obtained by PA1 contains sub-μM level Mg and Ca, which remarkably decrease matrix effect in ICP-MS analysis and significantly improve the analytical performance. With recovery better than 90% for most the trace metals examined, the accuracy was further verified through the analysis of five natural water reference materials with salinity spanning from 0 to 35‰. We have successfully applied the pretreatment system to determine trace metals in the seawater samples collected in the Western Philippine Sea through Taiwan GEOTRACES cruise. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. [Fluorescence Determination of Trace Se with the Hydride-K13-Rhodamine 6G System].

    PubMed

    Liang, Ai-hui; Li, Yuan; Huang, Shan-shan; Luo, Yang-he; Wen, Gui-qing; Jiang, Zhi-liang

    2015-05-01

    Se is a necessary trace element for human and animals, but the excess intake of Se caused poison. Thus, it is very important to determination of Se in foods and water. The target of this study is development of a new, sensitive and selective hydride generation-molecular fluorescence method for the determination of Se. In 0. 36 mol . L-1 sulfuric acid, NaBH4 as reducing agent, Se (IV) is reduced to H2 Se. Usin3-g I solution as absorption liquid3, I- is reduced to I- by H2Se. When adding rhodamine 6G, Rhodamine 6G and I3- form association particles, which lead to the fluorescence intensity decreased. When Se(IV) existing, Rhodamine 6G and I3- bind less, And the remaining amount of Rhodamine 6G increase. So the fluorescence intensity is enhanced. The analytical conditions were optimized, a 0. 36 ml . L-1 H2SO4, 21. 6.g . L-1 NaBH4, 23.3 µm . L-1 rhodamine 6G, and 50 µmol . L-1 KI3 were chosen for use. When the excitation wavelength is at 480nm, the Rayleigh scattering peak does not affect the fluorescence recording, and was selected for determination of Se. Under the selected conditions, Se(IV) concentration in the 0. 02~0. 60 µg . mL-1 range and the increase value of the fluorescence intensity (ΔF) at 562 nm linear relationship. The linear regression equation is ΔF562 nm =12. 6c + 20. 9. The detecton limit was 0.01 µ.g . L-1. The influence of coexistence substances on the hydride generatin-molecular fluorescence determination of 5. 07 X10(-6) mol . L-1 Se(IV) was considered in details. Results showed that this new fluorescence method is of high selectivity, that is, 0. 5 mmol. L-1 Ba2+, Ca2+, Zn2+ and Fe3+, 0. 25 mmol . L-1 . Mg2+, 0. 05 mmol . L-1 K+, 0. 2 mmol . L-1 Al3+, 0. 025 mmol . L-1 Te(VI) do not interfere with the determination. The influence of Hg2+, CD2+ and Cu2+ that precipitate with Se(IV), can be eliminated by addition of complex reagent. This hydride generation-molecular fluorescence method has been applied to determination of trace Se in water

  10. Trace Elements in River Waters

    NASA Astrophysics Data System (ADS)

    Gaillardet, J.; Viers, J.; Dupré, B.

    2003-12-01

    Trace elements are characterized by concentrations lower than 1 mg L-1 in natural waters. This means that trace elements are not considered when "total dissolved solids" are calculated in rivers, lakes, or groundwaters, because their combined mass is not significant compared to the sum of Na+, K+, Ca2+, Mg2+, H4SiO4, HCO3-, CO32-, SO42-, Cl-, and NO3-. Therefore, most of the elements, except about ten of them, occur at trace levels in natural waters. Being trace elements in natural waters does not necessarily qualify them as trace elements in rocks. For example, aluminum, iron, and titanium are major elements in rocks, but they occur as trace elements in waters, due to their low mobility at the Earth's surface. Conversely, trace elements in rocks such as chlorine and carbon are major elements in waters.The geochemistry of trace elements in river waters, like that of groundwater and seawater, is receiving increasing attention. This growing interest is clearly triggered by the technical advances made in the determination of concentrations at lower levels in water. In particular, the development of inductively coupled plasma mass spectrometry (ICP-MS) has considerably improved our knowledge of trace-element levels in waters since the early 1990s. ICP-MS provides the capability of determining trace elements having isotopes of interest for geochemical dating or tracing, even where their dissolved concentrations are extremely low.The determination of trace elements in natural waters is motivated by a number of issues. Although rare, trace elements in natural systems can play a major role in hydrosystems. This is particularly evident for toxic elements such as aluminum, whose concentrations are related to the abundance of fish in rivers. Many trace elements have been exploited from natural accumulation sites and used over thousands of years by human activities. Trace elements are therefore highly sensitive indexes of human impact from local to global scale. Pollution

  11. Dye tracing techniques used to determine ground-water flow in a carbonate aquifer system near Elizabethtown, Kentucky

    USGS Publications Warehouse

    Mull, D.S.; Smoot, J.L.; Liebermann, T.D.

    1988-01-01

    Because of the vulnerability of karst aquifers to contamination and the need for water managers to know recharge areas and groundwater flow characteristics for springs and wells used for public water supply, qualitative and quantitative dye tracing techniques were used during a groundwater investigation in the Elizabethtown area, Hardin County, in north-central Kentucky. The principal aquifer in the Elizabethtown area is thick, nearly horizontal beds of limestone, and thin beds of shale of Mississippi age. As much as 65% of all water pumped for the city water supply is obtained from two springs and two wells that obtain water from these rocks. Sinkholes were classified according to their ability to funnel runoff directly into the groundwater flow system, based primarily on the nature of the swallet draining the sinkhole. The presence of bedrock in the sinkhole nearly always ensured a well defined swallet leading to the subsurface. Qualitative and quantitative dye tracing techniques and equipment are discussed in detail. Qualitative dye tracing with fluorescein dye and passive dye detectors, consisting of activated coconut charcoal identified point to point connection between representative sinkholes, sinking streams, and karst windows and the city springs and wells. Qualitative tracing confirmed the presence of infiltrated surface water from a perennial stream, Valley Creek, in water from city wells and generally confirmed the direction of groundwater flow as shown by a water level contour map. Quantitative dye tracing with rhodamin WT, automatic samplers, discharge measurements, and fluorometric analyses were used to determine flow characteristics such as traveltime for arrival of the leading edge, peak concentration, trailing edge, and persistence of the dye cloud at the spring resurgence. Analyses of the dye recovery curves for quantitative dye traces completed between the same sinkholes and a city spring, and during different flow conditions showed that the

  12. Muon and Gamma Bundles tracing Up-going Tau Neutrino Astronomy

    NASA Astrophysics Data System (ADS)

    Fargion, D.; de Santis, M.; de Sanctis Lucentini, P. G.; Grossi, M.

    2004-11-01

    Up-going and Horizontal Tau Air-Showers, UpTaus and HorTaus, may trace Ultra High Energy Neutrino Tau Earth Skimming at the edge of the horizons. Their secondaries (μ± and γ bundles with e± pair flashes) might trace their nature over UHECR secondaries in horizontal showers. Indeed the atmosphere act as a perfect amplifier as well as a filter for showers: down-ward and horizontal μ bundles may still be originated by far Ultra High Energy Cosmic Rays skimming the terrestrial atmosphere but their rich gamma component will be exponentially suppressed. At large zenith angles after crossing a large slant depth (Xmax > 3 × 103 g cm-2) the number of μ± and secondary γ's (produced by the e± pair from μ decay in flight) is comparable. On the other hand, up-ward muon bundles from UpTaus and HorTaus may arise within a young shower with a larger gamma-muon ratio (˜ 102), leaving its characteristic imprint. We estimate the UpTaus and HorTaus rate from the Earth and we evaluate the consequent event rate of μ±, e± and γ bundles. We show that such events even for minimal GZK neutrino fluxes could be detected by scintillator arrays placed on mountains at 1 -5 km and pointing to the horizon. The required array areas are within tens-hundreds of square meters. An optimal structure is an array of crown-like twin detectors facing the horizons. We argue that such detectors will be able to detect both muonic bundles at a minimal average flux of 10-11 cm-2 s-1 sr-1 and electromagnetic particles (γ, e±) at 3 × 10-9 cm-2 s-1 sr-1, a few times each year, even for the minimal GZK ν flux.

  13. Trace conditioning in insects—keep the trace!

    PubMed Central

    Dylla, Kristina V.; Galili, Dana S.; Szyszka, Paul; Lüdke, Alja

    2013-01-01

    Trace conditioning is a form of associative learning that can be induced by presenting a conditioned stimulus (CS) and an unconditioned stimulus (US) following each other, but separated by a temporal gap. This gap distinguishes trace conditioning from classical delay conditioning, where the CS and US overlap. To bridge the temporal gap between both stimuli and to form an association between CS and US in trace conditioning, the brain must keep a neural representation of the CS after its termination—a stimulus trace. Behavioral and physiological studies on trace and delay conditioning revealed similarities between the two forms of learning, like similar memory decay and similar odor identity perception in invertebrates. On the other hand differences were reported also, like the requirement of distinct brain structures in vertebrates or disparities in molecular mechanisms in both vertebrates and invertebrates. For example, in commonly used vertebrate conditioning paradigms the hippocampus is necessary for trace but not for delay conditioning, and Drosophila delay conditioning requires the Rutabaga adenylyl cyclase (Rut-AC), which is dispensable in trace conditioning. It is still unknown how the brain encodes CS traces and how they are associated with a US in trace conditioning. Insects serve as powerful models to address the mechanisms underlying trace conditioning, due to their simple brain anatomy, behavioral accessibility and established methods of genetic interference. In this review we summarize the recent progress in insect trace conditioning on the behavioral and physiological level and emphasize similarities and differences compared to delay conditioning. Moreover, we examine proposed molecular and computational models and reassess different experimental approaches used for trace conditioning. PMID:23986710

  14. Age-related changes in ultra-triathlon performances

    PubMed Central

    2012-01-01

    Background The age-related decline in performance has been investigated in swimmers, runners and triathletes. No study has investigated the age-related performance decline in ultra-triathletes. The purpose of this study was to analyse the age-related declines in swimming, cycling, running and overall race time for both Triple Iron ultra-triathlon (11.4-km swimming, 540-km cycling and 126.6-km running) and Deca Iron ultra-triathlon (38-km swimming, 1,800-km cycling and 420-km running). Methods The age and performances of 423 male Triple Iron ultra-triathletes and 119 male Deca Iron ultra-triathletes were analysed from 1992 to 2010 using regression analyses and ANOVA. Results The mean age of the finishers was significantly higher for Deca Iron ultra-triathletes (41.3 ± 3.1 years) compared to a Triple Iron ultra-triathletes (38.5 ± 3.3 years) (P < 0.05). For both ultra-distances, the fastest overall race times were achieved between the ages of 25 and 44 years. Deca Iron ultra-triathletes achieved the same level of performance in swimming and cycling between 25 and 54 years of age. Conclusions The magnitudes of age-related declines in performance in the three disciplines of ultra-triathlon differ slightly between Triple and Deca Iron ultra-triathlon. Although the ages of Triple Iron ultra-triathletes were on average younger compared to Deca Iron ultra-triathletes, the fastest race times were achieved between 25 and 44 years for both distances. Further studies should investigate the motivation and training of ultra-triathletes to gain better insights in ultra-triathlon performance. PMID:23849327

  15. Accuracy of trace element determinations in alternate fuels

    NASA Technical Reports Server (NTRS)

    Greenbauer-Seng, L. A.

    1980-01-01

    A review of the techniques used at Lewis Research Center (LeRC) in trace metals analysis is presented, including the results of Atomic Absorption Spectrometry and DC Arc Emission Spectrometry of blank levels and recovery experiments for several metals. The design of an Interlaboratory Study conducted by LeRC is presented. Several factors were investigated, including: laboratory, analytical technique, fuel type, concentration, and ashing additive. Conclusions drawn from the statistical analysis will help direct research efforts toward those areas most responsible for the poor interlaboratory analytical results.

  16. Computer program for determination of concentrations of trace elements in components of water systems by nondestructive activation analysis (in German)

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

    Slavic, I.; Draskovic, R.; Tasovac, T.

    1973-03-01

    A computer program for the determination of trace elements in components of the water systems bed material, suspended material, dissolved substances, plankton, algae) by nondestructive activation analysis was developed. Results of the determination of Cr, Sb, Sc, Fe, Co, Na, and La concentrations in suspended materials from the Danube river, obtained by interpretation of data with a CDC- 3600 computer (64 k words), are presented. (auth)

  17. An R package for state-trace analysis.

    PubMed

    Prince, Melissa; Hawkins, Guy; Love, Jonathon; Heathcote, Andrew

    2012-09-01

    State-trace analysis (Bamber, Journal of Mathematical Psychology, 19, 137-181, 1979) is a graphical analysis that can determine whether one or more than one latent variable mediates an apparent dissociation between the effects of two experimental manipulations. State-trace analysis makes only ordinal assumptions and so, is not confounded by range effects that plague alternative methods, especially when performance is measured on a bounded scale (such as accuracy). We describe and illustrate the application of a freely available GUI driven package, StateTrace, for the R language. StateTrace automates many aspects of a state-trace analysis of accuracy and other binary response data, including customizable graphics and the efficient management of computationally intensive Bayesian methods for quantifying evidence about the outcomes of a state-trace experiment, developed by Prince, Brown, and Heathcote (Psychological Methods, 17, 78-99, 2012).

  18. Environmental factors determining the trace-level sorption of silver and thallium to soils.

    PubMed

    Jacobson, Astrid R; McBride, Murray B; Baveye, Philippe; Steenhuis, Tammo S

    2005-06-01

    Silver (Ag) and thallium (Tl) are nonessential elements that can be highly toxic to a number of biota even when present in the environment at trace levels. In spite of that, the literature on the chemistry and fate of Ag and Tl in soils is extremely scanty. In that context, the key objective of this research was to compare the sorption characteristics of trace amounts of Ag and Tl on a range of soils and minerals. A second objective was to determine the extent to which the composition and surface chemistry of the sorbents, as well as other environmental factors (simulated acid rain application and the presence of competing ions like K+ and NH4+) influence the sorption and lability of Ag and Tl. To this end, short-term and long-term sorption isotherms were generated under batch conditions for trace levels of Ag and Tl onto three illite-rich mineral soils from central New York (silt loam and fine sandy loam), a peaty-muck soil drained for agricultural use, and soil minerals (ferrihydrite and birnessite). Silver sorbed more strongly than thallium to all the soils. The peaty-muck soil sorbed Ag more strongly than the mineral soils, confirming that silver sorption to soils is dominated by soil organic matter either through exchange or complexation. The organic matter-rich soil's retention of Tl, however, was similar to that of the sandy soil. Amounts of Ag and Tl sorbed to the mineral soils increased after a 1-year incubation period. Whereas Ag sorption to the peaty-muck soil also increased with time, Tl sorption was unaffected. Short batch studies indicated that high amounts of Tl sorb to birnessite (30% by mass). However, subsequent X-ray diffraction (XRD) analysis of the solid did not detect the presence of any Tl3+ as Tl2O3 on the MnO4. In contrast, TlI was relatively poorly sorbed on noncrystalline ferrihydrite at pH 5.1 (1.5% by mass). Thus, Mn oxides may play a role in Tl retention by soils; whereas, contrary to previous reports, iron oxides do not effectively

  19. What predicts performance in ultra-triathlon races? – a comparison between Ironman distance triathlon and ultra-triathlon

    PubMed Central

    Knechtle, Beat; Zingg, Matthias Alexander; Rosemann, Thomas; Stiefel, Michael; Rüst, Christoph Alexander

    2015-01-01

    Objective This narrative review summarizes recent intentions to find potential predictor variables for ultra-triathlon race performance (ie, triathlon races longer than the Ironman distance covering 3.8 km swimming, 180 km cycling, and 42.195 km running). Results from studies on ultra-triathletes were compared to results on studies on Ironman triathletes. Methods A literature search was performed in PubMed using the terms “ultra”, “triathlon”, and “performance” for the aspects of “ultra-triathlon”, and “Ironman”, “triathlon”, and “performance” for the aspects of “Ironman triathlon”. All resulting papers were searched for related citations. Results for ultra-triathlons were compared to results for Ironman-distance triathlons to find potential differences. Results Athletes competing in Ironman and ultra-triathlon differed in anthropometric and training characteristics, where both Ironmen and ultra-triathletes profited from low body fat, but ultra-triathletes relied more on training volume, whereas speed during training was related to Ironman race time. The most important predictive variables for a fast race time in an ultra-triathlon from Double Iron (ie, 7.6 km swimming, 360 km cycling, and 84.4 km running) and longer were male sex, low body fat, age of 35–40 years, extensive previous experience, a fast time in cycling and running but not in swimming, and origins in Central Europe. Conclusion Any athlete intending to compete in an ultra-triathlon should be aware that low body fat and high training volumes are highly predictive for overall race time. Little is known about the physiological characteristics of these athletes and about female ultra-triathletes. Future studies need to investigate anthropometric and training characteristics of female ultra-triathletes and what motivates women to compete in these races. Future studies need to correlate physiological characteristics such as maximum oxygen uptake (VO2max) with ultra

  20. Physiology and Pathophysiology in Ultra-Marathon Running

    PubMed Central

    Knechtle, Beat; Nikolaidis, Pantelis T.

    2018-01-01

    In this overview, we summarize the findings of the literature with regards to physiology and pathophysiology of ultra-marathon running. The number of ultra-marathon races and the number of official finishers considerably increased in the last decades especially due to the increased number of female and age-group runners. A typical ultra-marathoner is male, married, well-educated, and ~45 years old. Female ultra-marathoners account for ~20% of the total number of finishers. Ultra-marathoners are older and have a larger weekly training volume, but run more slowly during training compared to marathoners. Previous experience (e.g., number of finishes in ultra-marathon races and personal best marathon time) is the most important predictor variable for a successful ultra-marathon performance followed by specific anthropometric (e.g., low body mass index, BMI, and low body fat) and training (e.g., high volume and running speed during training) characteristics. Women are slower than men, but the sex difference in performance decreased in recent years to ~10–20% depending upon the length of the ultra-marathon. The fastest ultra-marathon race times are generally achieved at the age of 35–45 years or older for both women and men, and the age of peak performance increases with increasing race distance or duration. An ultra-marathon leads to an energy deficit resulting in a reduction of both body fat and skeletal muscle mass. An ultra-marathon in combination with other risk factors, such as extreme weather conditions (either heat or cold) or the country where the race is held, can lead to exercise-associated hyponatremia. An ultra-marathon can also lead to changes in biomarkers indicating a pathological process in specific organs or organ systems such as skeletal muscles, heart, liver, kidney, immune and endocrine system. These changes are usually temporary, depending on intensity and duration of the performance, and usually normalize after the race. In longer ultra

  1. Physiology and Pathophysiology in Ultra-Marathon Running.

    PubMed

    Knechtle, Beat; Nikolaidis, Pantelis T

    2018-01-01

    In this overview, we summarize the findings of the literature with regards to physiology and pathophysiology of ultra-marathon running. The number of ultra-marathon races and the number of official finishers considerably increased in the last decades especially due to the increased number of female and age-group runners. A typical ultra-marathoner is male, married, well-educated, and ~45 years old. Female ultra-marathoners account for ~20% of the total number of finishers. Ultra-marathoners are older and have a larger weekly training volume, but run more slowly during training compared to marathoners. Previous experience (e.g., number of finishes in ultra-marathon races and personal best marathon time) is the most important predictor variable for a successful ultra-marathon performance followed by specific anthropometric (e.g., low body mass index, BMI, and low body fat) and training (e.g., high volume and running speed during training) characteristics. Women are slower than men, but the sex difference in performance decreased in recent years to ~10-20% depending upon the length of the ultra-marathon. The fastest ultra-marathon race times are generally achieved at the age of 35-45 years or older for both women and men, and the age of peak performance increases with increasing race distance or duration. An ultra-marathon leads to an energy deficit resulting in a reduction of both body fat and skeletal muscle mass. An ultra-marathon in combination with other risk factors, such as extreme weather conditions (either heat or cold) or the country where the race is held, can lead to exercise-associated hyponatremia. An ultra-marathon can also lead to changes in biomarkers indicating a pathological process in specific organs or organ systems such as skeletal muscles, heart, liver, kidney, immune and endocrine system. These changes are usually temporary, depending on intensity and duration of the performance, and usually normalize after the race. In longer ultra

  2. [Determination of trace elements in waste beer yeasts by ICP-MS with microwave digestion].

    PubMed

    Cheng, Xian-zhong; Jin, Can; Zhang, Kai-cheng

    2008-10-01

    The waste beer yeast has rich nutritional compositions and is widely used in food, medical and forage industries. The security of the yeast plays an important role in everyone's daily life. But the yeast contanining microamount of lead, cadmium, chromium, arsenic and other harmful metals is endangering human health. A new method was developed for the direct determination of eight elements, namely copper, lead, zinc, iron, manganese, cadmium, chromium and arsenic in waste beer yeast by inductively coupled plasma-mass spectrometry (ICP-MS) with microwave digestion. The parameters of plasma system, mass system, vacuum system and spectrometer system were optimized. The spectral interferences were eliminated by selecting alternation analytical isotopes of 65Cu, 208Pb, 66Zn, 57Fe, 55Mn, 114Cd, 52Cr and 5As, and the internal standards of Rh was selected to compensate the drift of analytical signals. The samples were digested with concentrated nitric acid-hydrogen peroxide (2:1) mixed solution more rapidly and more effectively. The effects of the type of mixed acid , the volume of digesting solution, heating time, and heating power were investigated in detail. In the closed system, the complete digestion was performed using 4 mL HNO3 and 2mL H2O2 for 2.0 min at 0.5 MPa, 3 min at 1.0 MPa and 5 min at 1.5 MPa. The detection limits of these eight elements were 0.013-0.122 microg x L(-1). The relative standard deviation (RSD) was 0.94%-3.26% (n=9), and the addition standard recovery was 98.4%-102.6% for all elements. The proposed method has been applied to the determination of trace elements of Cu, Pb, Zn, Fe, Mn, Cd, Cr and As in waste beer yeast samples with satisfactory results. The determination results indicated that the content of trace elements of Cu, Pb, Cd and As in waste beer yeast samples are significantly low.

  3. Pump-probe micro-spectroscopy by means of an ultra-fast acousto-optics delay line.

    PubMed

    Audier, Xavier; Balla, Naveen; Rigneault, Hervé

    2017-01-15

    We demonstrate femtosecond pump-probe transient absorption spectroscopy using a programmable dispersive filter as an ultra-fast delay line. Combined with fast synchronous detection, this delay line allows for recording of 6 ps decay traces at 34 kHz. With such acquisition speed, we perform single point pump-probe spectroscopy on bulk samples in 80 μs and hyperspectral pump-probe imaging over a field of view of 100 μm in less than a second. The usability of the method is illustrated in a showcase experiment to image and discriminate between two pigments in a mixture.

  4. Pulsed 86Sr-labeling and NanoSIMS imaging to study coral biomineralization at ultra-structural length scales

    NASA Astrophysics Data System (ADS)

    Brahmi, C.; Domart-Coulon, I.; Rougée, L.; Pyle, D. G.; Stolarski, J.; Mahoney, J. J.; Richmond, R. H.; Ostrander, G. K.; Meibom, A.

    2012-09-01

    A method to label marine biocarbonates is developed based on a concentration enrichment of a minor stable isotope of a trace element that is a natural component of seawater, resulting in the formation of biocarbonate with corresponding isotopic enrichments. This biocarbonate is subsequently imaged with a NanoSIMS ion microprobe to visualize the locations of the isotopic marker on sub-micrometric length scales, permitting resolution of all ultra-structural details. In this study, a scleractinian coral, Pocillopora damicornis, was labeled 3 times with 86Sr-enhanced seawater for a period of 48 h with 5 days under normal seawater conditions separating each labeling event. Two non-specific cellular stress biomarkers, glutathione-S-transferase activity and porphyrin concentration plus carbonic anhydrase, an enzymatic marker involved in the physiology of carbonate biomineralization, as well as unchanged levels of zooxanthellae photosynthesis efficiency indicate that coral physiological processes are not affected by the 86Sr-enhancement. NanoSIMS images of the 86Sr/44Ca ratio in skeleton formed during the experiment allow for a determination of the average extension rate of the two major ultra-structural components of the coral skeleton: Rapid Accretion Deposits are found to form on average about 4.5 times faster than Thickening Deposits. The method opens up new horizons in the study of biocarbonate formation because it holds the potential to observe growth of calcareous structures such as skeletons, shells, tests, spines formed by a wide range of organisms under essentially unperturbed physiological conditions.

  5. Spectroscopic Determination of Trace Contaminants in High Purity Oxygen

    NASA Technical Reports Server (NTRS)

    Hornung, Steven D.

    2011-01-01

    Oxygen used for extravehicular activities (EVA) must be free of contaminants because a difference in a few tenths of a percent of argon or nitrogen content can mean significant reduction in available EVA time. These inert gases build up in the extravehicular mobility unit because they are not metabolized or scrubbed from the atmosphere. Measurement of oxygen purity above 99.5% is problematic, and currently only complex instruments such as gas chromatographs or mass spectrometers are used for these determinations. Because liquid oxygen boil-off from the space shuttle will no longer be available to supply oxygen for EVA use, other concepts are being developed to produce and validate high purity oxygen from cabin air aboard the International Space Station. A prototype optical emission technique capable of detecting argon and nitrogen below 0.1% in oxygen was developed at White Sands Test Facility. This instrument uses a glow discharge in reduced pressure gas to produce atomic emission from the species present. Because the atomic emission lines from oxygen, nitrogen, and argon are discrete and in many cases well-separated, trace amounts of argon and nitrogen can be detected in the ultraviolet and visible spectrum. This is a straightforward, direct measurement of the target contaminants and may lend itself to a device capable of on-orbit verification of oxygen purity. System design and optimized measurement parameters are presented.

  6. Simultaneous determination of trace rare-earth elements in simulated water samples using ICP-OES with TODGA extraction/back-extraction.

    PubMed

    Li, FuKai; Gong, AiJun; Qiu, LiNa; Zhang, WeiWei; Li, JingRui; Liu, Yu; Liu, YuNing; Yuan, HuiTing

    2017-01-01

    The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N', N'-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4-1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples.

  7. Advanced functional materials in solid phase extraction for ICP-MS determination of trace elements and their species - A review.

    PubMed

    He, Man; Huang, Lijin; Zhao, Bingshan; Chen, Beibei; Hu, Bin

    2017-06-22

    For the determination of trace elements and their species in various real samples by inductively coupled plasma mass spectrometry (ICP-MS), solid phase extraction (SPE) is a commonly used sample pretreatment technique to remove complex matrix, pre-concentrate target analytes and make the samples suitable for subsequent sample introduction and measurements. The sensitivity, selectivity/anti-interference ability, sample throughput and application potential of the methodology of SPE-ICP-MS are greatly dependent on SPE adsorbents. This article presents a general overview of the use of advanced functional materials (AFMs) in SPE for ICP-MS determination of trace elements and their species in the past decade. Herein the AFMs refer to the materials featuring with high adsorption capacity, good selectivity, fast adsorption/desorption dynamics and satisfying special requirements in real sample analysis, including nanometer-sized materials, porous materials, ion imprinting polymers, restricted access materials and magnetic materials. Carbon/silica/metal/metal oxide nanometer-sized adsorbents with high surface area and plenty of adsorption sites exhibit high adsorption capacity, and porous adsorbents would provide more adsorption sites and faster adsorption dynamics. The selectivity of the materials for target elements/species can be improved by using physical/chemical modification, ion imprinting and restricted accessed technique. Magnetic adsorbents in conventional batch operation offer unique magnetic response and high surface area-volume ratio which provide a very easy phase separation, greater extraction capacity and efficiency over conventional adsorbents, and chip-based magnetic SPE provides a versatile platform for special requirement (e.g. cell analysis). The performance of these adsorbents for the determination of trace elements and their species in different matrices by ICP-MS is discussed in detail, along with perspectives and possible challenges in the future

  8. Simultaneous determination of trace rare-earth elements in simulated water samples using ICP-OES with TODGA extraction/back-extraction

    PubMed Central

    Li, FuKai; Qiu, LiNa; Zhang, WeiWei; Li, JingRui; Liu, Yu; Liu, YuNing; Yuan, HuiTing

    2017-01-01

    The determination of trace rare-earth elements (REEs) can be used for the assessment of environmental pollution, and is of great significance to the study of toxicity and toxicology in animals and plants. N, N, N′, N′-tetraoctyl diglycolamide (TODGA) is an environmental friendly extractant that is highly selective to REEs. In this study, an analytical method was developed for the simultaneous determination of 16 trace REEs in simulated water samples by inductively coupled plasma optical emission spectroscopy (ICP-OES). With this method, TODGA was used as the extractant to perform the liquid-liquid extraction (LLE) sample pretreatment procedure. All 16 REEs were extracted from a 3 M nitric acid medium into an organic phase by a 0.025 M TODGA petroleum ether solution. A 0.03 M ethylenediaminetetraacetic acid disodium salt (EDTA) solution was used for back-extraction to strip the REEs from the organic phase into the aqueous phase. The aqueous phase was concentrated using a vacuum rotary evaporator and the concentration of the 16 REEs was detected by ICP-OES. Under the optimum experimental conditions, the limits of detection (3σ, n = 7) for the REEs ranged from 0.0405 ng mL-1 (Nd) to 0.5038 ng mL-1 (Ho). The relative standard deviations (c = 100 ng mL-1, n = 7) were from 0.5% (Eu) to 4.0% (Tm) with a linear range of 4–1000 ng mL-1 (R2 > 0.999). The recoveries of 16 REEs ranged from 95% to 106%. The LLE-ICP-OES method established in this study has the advantages of simple operation, low detection limits, fast analysis speed and the ability to simultaneously determine 16 REEs, thereby acting as a viable alternative for the simultaneous detection of trace amounts of REEs in water samples. PMID:28945788

  9. [Determination of trace amounts of zinc in nickel electrolyte by flow injection on-line enrichment].

    PubMed

    Zhou, Z; Wang, Y; Dong, Z; Tong, K; Guo, X; Guo, X

    1999-10-01

    A method for the determination of trace amount of zinc in nickel electrolyte utilizing the flow injection on-line enrichment technique is reported in this paper. Atomic absorption spectrometer was used as detector. Zinc was separated from large amounts of nickel andother components in the electrolyte by absorption its chlorocomplex on a mini-column packed with strongly basic anion exchangers. It was found that sodium chloride containing in the electrolyte offered a sufficient chloride concentration needed for the formation of the zinc chlorocomplex and thus no additional reagent was required for the determination. The throughput of the method is 30 determinations per hour. The detection limit of the method is 0.002 microg x mL(-1) and the precision is 1.9% (RSD). The proposed method is rapid and cost-effective. It has been used for almost three years in the quality control of the electrolyte in the factory with great success.

  10. Temporally rendered automatic cloud extraction (TRACE) system

    NASA Astrophysics Data System (ADS)

    Bodrero, Dennis M.; Yale, James G.; Davis, Roger E.; Rollins, John M.

    1999-10-01

    Smoke/obscurant testing requires that 2D cloud extent be extracted from visible and thermal imagery. These data are used alone or in combination with 2D data from other aspects to make 3D calculations of cloud properties, including dimensions, volume, centroid, travel, and uniformity. Determining cloud extent from imagery has historically been a time-consuming manual process. To reduce time and cost associated with smoke/obscurant data processing, automated methods to extract cloud extent from imagery were investigated. The TRACE system described in this paper was developed and implemented at U.S. Army Dugway Proving Ground, UT by the Science and Technology Corporation--Acuity Imaging Incorporated team with Small Business Innovation Research funding. TRACE uses dynamic background subtraction and 3D fast Fourier transform as primary methods to discriminate the smoke/obscurant cloud from the background. TRACE has been designed to run on a PC-based platform using Windows. The PC-Windows environment was chosen for portability, to give TRACE the maximum flexibility in terms of its interaction with peripheral hardware devices such as video capture boards, removable media drives, network cards, and digital video interfaces. Video for Windows provides all of the necessary tools for the development of the video capture utility in TRACE and allows for interchangeability of video capture boards without any software changes. TRACE is designed to take advantage of future upgrades in all aspects of its component hardware. A comparison of cloud extent determined by TRACE with manual method is included in this paper.

  11. [The study of ultra-fine diamond powder used in magnetic head polishing slurry].

    PubMed

    Jin, Hong-Yun; Hou, Shu-En; Pan, Yong; Xiao, Hong-Yan

    2008-05-01

    In the present paper, atomic absorption spectrometry(AAS), inductively-coupled plasma mass spectrometry (ICP-MS), transmission electron microscopy (TEM), X-ray diffraction (XRD) and laser Raman spectroscopy (RM) were employed to study the commercial ultra-fine diamond powders prepared by the static pressure-catalyst method and used in magnetic head polishing slurry. The results of AAS and ICP-MS indicated that there were silicon oxide, Fe, Ni, Al and some other metal elements in the ultra-fine powders. XRD patterns showed the peaks of SiO2 at 2theta = 35.6 degrees, 39.4 degrees and 59.7 degrees and diamond sharp peaks in agreement with the results above. Diamond sharp peaks implied perfect crystal and high-hardness beneficial to high-efficiency in polishing. The broader Raman band of graphite at 1 592 cm(-1) observed by Raman analysis proved graphite existing in the diamond powders. In the TEM images, the size of ultra-fine powders was estimated between 0.1 and 0.5 microm distributed in a wide scope, however, sharp edges of the powder particles was useful to polish. The ultra-fine diamond powders have many advantages, for example, high-hardness, well abrasion performance, high-polishing efficiency and being useful in magnetic head polishing slurry. But, the impurities influence the polishing efficiency, shortening its service life and the wide distribution reduces the polishing precision. Consequently, before use the powders must be purified and classified. The purity demands is 99.9% and trace silicon oxide under 0.01% should be reached. The classification demands that the particle distribution should be in a narrower scope, with the mean size of 100 nm and the percentage of particles lager than 200 nm not over 2%.

  12. Analytical Methods for Trace Metals. Training Manual.

    ERIC Educational Resources Information Center

    Office of Water Program Operations (EPA), Cincinnati, OH. National Training and Operational Technology Center.

    This training manual presents material on the theoretical concepts involved in the methods listed in the Federal Register as approved for determination of trace metals. Emphasis is on laboratory operations. This course is intended for chemists and technicians with little or no experience in analytical methods for trace metals. Students should have…

  13. SXRF determination of trace elements in chondrule rims in the unequilibrated CO3 chondrite, ALH A77307

    NASA Technical Reports Server (NTRS)

    Brearley, Adrian J.; Bajt, Sasa; Sutton, Steve R.; Papike, J. J.

    1993-01-01

    The concentrations of Ni, Cu, Zn, Ga, Ge, and Se in five chondrule rims in the CO3 chondrite ALH A77307 (3.0) using the synchrotron x-ray fluorescence (SXRF) microprobe at Brookhaven National Laboratory were determined. The data show that the trace element chemistry of rims on different chondrules is remarkably similar, consistent with data obtained for the major elements by electron microprobe. These results support the idea that rims are not genetically related to individual chondrules, but all sampled the same reservoir of homogeneously mixed dust. Of the trace elements analyzed Zn and Ga show depletions relative to CI chondrite values, but in comparison with bulk CO chondrites all the elements are enriched by approximately 1.5 to 3.5 x CO. The high concentrations of the highly volatile elements Se and Ga and moderately volatile Zn (1.5 to 2 x CO) in rims show that matrix is the major reservoir of volatile elements in ALH A77307.

  14. Electrochemical Determination of Trace Sudan I Contamination in Chili Powder at Carbon Nanotube Modified Electrodes

    PubMed Central

    Ming, Liang; Xi, Xia; Chen, Tingting; Liu, Jie

    2008-01-01

    We have developed a simple, convenient and inexpensive voltammetric method for determining trace Sudan I contamination in chili powder, based on the catalyzed electrochemical reduction of Sudan I at the carbon nanotube modified electrode. Under optimized conditions, the method exhibited acceptable analytical performance in terms of linearity (over the concentration range 6.0×10−7 to 7.5×10−5 M, r = 0.9967), detection limit (2.0×10−7 M) and reproducibility (RSD = 4.6%, n=10, for 2.0×10−5 M Sudan I). PMID:27879800

  15. Evaluation of the UV/H2O2 system for treating natural water with a mixture of anthracene and benzo[a]pyrene at ultra-trace levels.

    PubMed

    Rubio-Clemente, Ainhoa; Chica, Edwin; Peñuela, Gustavo

    2018-06-05

    The presence of polycyclic aromatic hydrocarbons, such as anthracene (AN) and benzo[a]pyrene (BaP), in water has become a problem of great concern due to the detrimental health effects caused to humans and living beings. In this work, the efficiency of the UV/H 2 O 2 system for degrading the target compounds at ultra-trace levels in surface water has been evaluated. For this purpose, a previous optimization step using a face-centered central composite experimental design has been conducted, considering the effect of the UV-C irradiance and the initial concentration of H 2 O 2 . It was evidenced that under optimal operating conditions (11 mg L -1 H 2 O 2 and 0.63 mW cm -2 irradiance), AN and BaP removal percentages were higher than 99.8%. Additionally, 69.3% of the organic matter, in terms of total organic carbon, was mineralized without the production of transformation by-products more harmful than the parent compounds. These findings demonstrate the oxidation capacity of the examined system in a natural matrix for degrading micropollutants that cannot be converted through conventional treatment processes. Consequently, new horizons are opened for the effective use of the UV/H 2 O 2 system for drinking water production, providing the accomplishment of other regulated parameters related to water quality.

  16. Use of chiral derivatization for the determination of dichlorprop in tea samples by ultra performance LC with fluorescence detection.

    PubMed

    Inoue, Koichi; Prayoonhan, Nuntawat; Tsutsui, Haruhito; Sakamoto, Tasuku; Nishimura, Maiko; Toyo'oka, Toshimasa

    2013-04-01

    Dichlorprop is available for agricultural use as a chiral pesticide. In this study, the stereoselective determination of dichlorprop enantiomers in tea samples such as green, black, jasmine, and oolong was developed by ultra performance LC with fluorescence spectrometry after covalent chiral derivatization. The separation was achieved on an Acquity BEH C18 column with the mobile phase consisting of 0.1% formic acid in acetonitrile/water at a flow rate of 0.4 mL/min. In the covalent chiral derivatization using (S)-(+)-4-(N,N-dimethylaminosulfonyl)-7-(3-aminopyrrolidin-1-yl)-2,1,3-benzoxadiazole, the peak resolution between the S and R-dichlorprop enantiomers was 2.6. LODs and LOQs values were 10 and 50 ng/mL standard solution. The linearity of the calibration curves yielded the coefficients (r(2) > 0.99, ranging from 0.05 to 5 μg/mL) of determination of each of the dichlorprop enantiomers. SPE extraction was used for the sample preparation of dichlorprop in various tea samples. Recoveries were in the range of 82.4-97.6% with associated precision values (within-day: 82.4-95.8%, n = 6, and between-day: 83.7-97.6% for 3 days) for repeatability and reproducibility. Based on this result, our method has been proven to be highly efficient and suitable for the routine assay of dichlorprop enantiomers in various tea samples. We propose that the ultra performance LC assay after covalent chiral derivatization would be the renewed tools in the era of chiral stationary platform for chiral pesticide residues in foods. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Formal thought disorder in people at ultra-high risk of psychosis

    PubMed Central

    Weinstein, Sara; Stahl, Daniel; Day, Fern; Valmaggia, Lucia; Rutigliano, Grazia; De Micheli, Andrea; Fusar-Poli, Paolo; McGuire, Philip

    2017-01-01

    Background Formal thought disorder is a cardinal feature of psychosis. However, the extent to which formal thought disorder is evident in ultra-high-risk individuals and whether it is linked to the progression to psychosis remains unclear. Aims Examine the severity of formal thought disorder in ultra-high-risk participants and its association with future psychosis. Method The Thought and Language Index (TLI) was used to assess 24 ultra-high-risk participants, 16 people with first-episode psychosis and 13 healthy controls. Ultra-high-risk individuals were followed up for a mean duration of 7 years (s.d.=1.5) to determine the relationship between formal thought disorder at baseline and transition to psychosis. Results TLI scores were significantly greater in the ultra-high-risk group compared with the healthy control group (effect size (ES)=1.2), but lower than in people with first-episode psychosis (ES=0.8). Total and negative TLI scores were higher in ultra-high-risk individuals who developed psychosis, but this was not significant. Combining negative TLI scores with attenuated psychotic symptoms and basic symptoms predicted transition to psychosis (P=0.04; ES=1.04). Conclusions TLI is beneficial in evaluating formal thought disorder in ultra-high-risk participants, and complements existing instruments for the evaluation of psychopathology in this group. Declaration of interests None. Copyright and usage © The Royal College of Psychiatrists 2017. This is an open access article distributed under the terms of the Creative Commons Non-Commercial, No Derivatives (CC BY-NC-ND) license. PMID:28713586

  18. Ultra-processed Food Intake and Obesity: What Really Matters for Health-Processing or Nutrient Content?

    PubMed

    Poti, Jennifer M; Braga, Bianca; Qin, Bo

    2017-12-01

    The aim of this narrative review was to summarize and critique recent evidence evaluating the association between ultra-processed food intake and obesity. Four of five studies found that higher purchases or consumption of ultra-processed food was associated with overweight/obesity. Additional studies reported relationships between ultra-processed food intake and higher fasting glucose, metabolic syndrome, increases in total and LDL cholesterol, and risk of hypertension. It remains unclear whether associations can be attributed to processing itself or the nutrient content of ultra-processed foods. Only three of nine studies used a prospective design, and the potential for residual confounding was high. Recent research provides fairly consistent support for the association of ultra-processed food intake with obesity and related cardiometabolic outcomes. There is a clear need for further studies, particularly those using longitudinal designs and with sufficient control for confounding, to potentially confirm these findings in different populations and to determine whether ultra-processed food consumption is associated with obesity independent of nutrient content.

  19. Photoresponsive molecularly imprinted hydrogel casting membrane for the determination of trace tetracycline in milk.

    PubMed

    Wang, Qiang; Lv, Zhen; Tang, Qian; Gong, Cheng-Bin; Lam, Michael Hon Wah; Ma, Xue-Bing; Chow, Cheuk-Fai

    2016-03-01

    This study aimed to develop a photoresponsive molecularly imprinted hydrogel (MIH) casting membrane for the determination of trace tetracycline (TC) in milk. This MIH casting membrane combined the specificity of MIHs, the photoresponsive properties of azobenzene, and the portable properties of a membrane. Photoresponsive TC-imprinted MIHs were initially fabricated and then cast on sodium dodecyl sulfonate polyacrylamide gel. After TC removal, a photoresponsive MIH casting membrane was obtained. The photoresponsive properties of the MIH casting membrane were robust, and no obvious photodegradation was observed after 20 cycles. The MIH casting membrane displayed specific affinity to TC upon alternate irradiation at 365 and 440 nm; it could quantitatively uptake and release TC. The TC concentration (0.0-2.0 × 10(-4) mol l(-1)) in aqueous solution displayed a linear relationship with the photoisomerization rate constant of azobenzene within the MIH casting membrane. As such, a quick detection method for trace TC in aqueous foodstuff samples was established. The recovery of this method for TC in milk was investigated with a simple pretreatment of milk, and a high recovery of 100.54-106.35% was obtained. Therefore, the fabricated membrane can be used as a portable molecular sensor that can be easily recycled. Copyright © 2015 John Wiley & Sons, Ltd.

  20. Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

    NASA Astrophysics Data System (ADS)

    de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

    2014-06-01

    An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

  1. Consumers' conceptualization of ultra-processed foods.

    PubMed

    Ares, Gastón; Vidal, Leticia; Allegue, Gimena; Giménez, Ana; Bandeira, Elisa; Moratorio, Ximena; Molina, Verónika; Curutchet, María Rosa

    2016-10-01

    Consumption of ultra-processed foods has been associated with low diet quality, obesity and other non-communicable diseases. This situation makes it necessary to develop educational campaigns to discourage consumers from substituting meals based on unprocessed or minimally processed foods by ultra-processed foods. In this context, the aim of the present work was to investigate how consumers conceptualize the term ultra-processed foods and to evaluate if the foods they perceive as ultra-processed are in concordance with the products included in the NOVA classification system. An online study was carried out with 2381 participants. They were asked to explain what they understood by ultra-processed foods and to list foods that can be considered ultra-processed. Responses were analysed using inductive coding. The great majority of the participants was able to provide an explanation of what ultra-processed foods are, which was similar to the definition described in the literature. Most of the participants described ultra-processed foods as highly processed products that usually contain additives and other artificial ingredients, stressing that they have low nutritional quality and are unhealthful. The most relevant products for consumers' conceptualization of the term were in agreement with the NOVA classification system and included processed meats, soft drinks, snacks, burgers, powdered and packaged soups and noodles. However, some of the participants perceived processed foods, culinary ingredients and even some minimally processed foods as ultra-processed. This suggests that in order to accurately convey their message, educational campaigns aimed at discouraging consumers from consuming ultra-processed foods should include a clear definition of the term and describe some of their specific characteristics, such as the type of ingredients included in their formulation and their nutritional composition. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Method for remote detection of trace contaminants

    DOEpatents

    Simonson, Robert J.; Hance, Bradley G.

    2003-09-09

    A method for remote detection of trace contaminants in a target area comprises applying sensor particles that preconcentrate the trace contaminant to the target area and detecting the contaminant-sensitive fluorescence from the sensor particles. The sensor particles can have contaminant-sensitive and contaminant-insensitive fluorescent compounds to enable the determination of the amount of trace contaminant present in the target are by relative comparison of the emission of the fluorescent compounds by a local or remote fluorescence detector. The method can be used to remotely detect buried minefields.

  3. Procedures of determining organic trace compounds in municipal sewage sludge-a review.

    PubMed

    Lindholm-Lehto, Petra C; Ahkola, Heidi S J; Knuutinen, Juha S

    2017-02-01

    Sewage sludge is the largest by-product generated during the wastewater treatment process. Since large amounts of sludge are being produced, different ways of disposal have been introduced. One tempting option is to use it as fertilizer in agricultural fields due to its high contents of inorganic nutrients. This, however, can be limited by the amount of trace contaminants in the sewage sludge, containing a variety of microbiological pollutants and pathogens but also inorganic and organic contaminants. The bioavailability and the effects of trace contaminants on the microorganisms of soil are still largely unknown as well as their mixture effects. Therefore, there is a need to analyze the sludge to test its suitability before further use. In this article, a variety of sampling, pretreatment, extraction, and analysis methods have been reviewed. Additionally, different organic trace compounds often found in the sewage sludge and their methods of analysis have been compiled. In addition to traditional Soxhlet extraction, the most common extraction methods of organic contaminants in sludge include ultrasonic extraction (USE), supercritical fluid extraction (SFE), microwave-assisted extraction (MAE), and pressurized liquid extraction (PLE) followed by instrumental analysis based on gas or liquid chromatography and mass spectrometry.

  4. Development of an Ultra-Low Background Liquid Scintillation Counter for Trace Level Analysis

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

    Erchinger, Jennifer L.; Orrell, John L.; Aalseth, Craig E.

    2015-09-01

    Low-level liquid scintillation counting (LSC) has been established as one of the radiation detection techniques useful in elucidating environmental processes and environmental monitoring around nuclear facilities. The Ultra-Low Background Liquid Scintillation Counter (ULB-LSC) under construction in the Shallow Underground Laboratory at Pacific Northwest National Laboratory aims to further reduce the MDAs and/or required sample processing. Through layers of passive shielding in conjunction with an active veto and 30 meters water equivalent overburden, the background reduction is expected to be 10 to 100 times below typical analytic low-background liquid scintillation systems. Simulations have shown an expected background of around 14 countsmore » per day. A novel approach to the light collection will use a coated hollow light guide cut into the inner copper shielding. Demonstration LSC measurements will show low-energy detection, spectral deconvolution, and alpha/beta discrimination capabilities, from trials with standards of tritium, strontium-90, and actinium-227, respectively. An overview of the system design and expected demonstration measurements will emphasize the potential applications of the ULB-LSC in environmental monitoring for treaty verification, reach-back sample analysis, and facility inspections.« less

  5. Development of a selective and sensitive flotation method for determination of trace amounts of cobalt, nickel, copper and iron in environmental samples.

    PubMed

    Karimi, H; Ghaedi, M; Shokrollahi, A; Rajabi, H R; Soylak, M; Karami, B

    2008-02-28

    A simple, selective and rapid flotation method for the separation-preconcentration of trace amounts of cobalt, nickel, iron and copper ions using phenyl 2-pyridyl ketone oxime (PPKO) has been developed prior to their flame atomic absorption spectrometric determinations. The influence of pH, amount of PPKO as collector, type and amount of eluting agent, type and amount of surfactant as floating agent and ionic strength was evaluated on the recoveries of analytes. The influences of the concomitant ions on the recoveries of the analyte ions were also examined. The enrichment factor was 93. The detection limits based on 3 sigma for Cu, Ni, Co and Fe were 0.7, 0.7, 0.8, and 0.7 ng mL(-1), respectively. The method has been successfully applied for determination of trace amounts of ions in various real samples.

  6. Weighing Ultra-Cool Stars

    NASA Astrophysics Data System (ADS)

    2004-05-01

    Large Ground-Based Telescopes and Hubble Team-Up to Perform First Direct Brown Dwarf Mass Measurement [1] Summary Using ESO's Very Large Telescope at Paranal and a suite of ground- and space-based telescopes in a four-year long study, an international team of astronomers has measured for the first time the mass of an ultra-cool star and its companion brown dwarf. The two stars form a binary system and orbit each other in about 10 years. The team obtained high-resolution near-infrared images; on the ground, they defeated the blurring effect of the terrestrial atmosphere by means of adaptive optics techniques. By precisely determining the orbit projected on the sky, the astronomers were able to measure the total mass of the stars. Additional data and comparison with stellar models then yield the mass of each of the components. The heavier of the two stars has a mass around 8.5% of the mass of the Sun and its brown dwarf companion is even lighter, only 6% of the solar mass. Both objects are relatively young with an age of about 500-1,000 million years. These observations represent a decisive step towards the still missing calibration of stellar evolution models for very-low mass stars. PR Photo 19a/04: Orbit of the ultra-cool stars in 2MASSW J0746425+2000321. PR Photo 19b/04: Animated Gif of the orbital motion. Telephone number star Even though astronomers have found several hundreds of very low mass stars and brown dwarfs, the fundamental properties of these extreme objects, such as masses and surface temperatures, are still not well known. Within the cosmic zoo, these ultra-cool stars represent a class of "intermediate" objects between giant planets - like Jupiter - and "normal" stars less massive than our Sun, and to understand them well is therefore crucial to the field of stellar astrophysics. The problem with these ultra-cool stars is that contrary to normal stars that burn hydrogen in their central core, no unique relation exists between the luminosity of the

  7. Trace Elements in Ovaries: Measurement and Physiology.

    PubMed

    Ceko, Melanie J; O'Leary, Sean; Harris, Hugh H; Hummitzsch, Katja; Rodgers, Raymond J

    2016-04-01

    Traditionally, research in the field of trace element biology and human and animal health has largely depended on epidemiological methods to demonstrate involvement in biological processes. These studies were typically followed by trace element supplementation trials or attempts at identification of the biochemical pathways involved. With the discovery of biological molecules that contain the trace elements, such as matrix metalloproteinases containing zinc (Zn), cytochrome P450 enzymes containing iron (Fe), and selenoproteins containing selenium (Se), much of the current research focuses on these molecules, and, hence, only indirectly on trace elements themselves. This review focuses largely on two synchrotron-based x-ray techniques: X-ray absorption spectroscopy and x-ray fluorescence imaging that can be used to identify the in situ speciation and distribution of trace elements in tissues, using our recent studies of bovine ovaries, where the distribution of Fe, Se, Zn, and bromine were determined. It also discusses the value of other techniques, such as inductively coupled plasma mass spectrometry, used to garner information about the concentrations and elemental state of the trace elements. These applications to measure trace elemental distributions in bovine ovaries at high resolutions provide new insights into possible roles for trace elements in the ovary. © 2016 by the Society for the Study of Reproduction, Inc.

  8. Deep learning and shapes similarity for joint segmentation and tracing single neurons in SEM images

    NASA Astrophysics Data System (ADS)

    Rao, Qiang; Xiao, Chi; Han, Hua; Chen, Xi; Shen, Lijun; Xie, Qiwei

    2017-02-01

    Extracting the structure of single neurons is critical for understanding how they function within the neural circuits. Recent developments in microscopy techniques, and the widely recognized need for openness and standardization provide a community resource for automated reconstruction of dendritic and axonal morphology of single neurons. In order to look into the fine structure of neurons, we use the Automated Tape-collecting Ultra Microtome Scanning Electron Microscopy (ATUM-SEM) to get images sequence of serial sections of animal brain tissue that densely packed with neurons. Different from other neuron reconstruction method, we propose a method that enhances the SEM images by detecting the neuronal membranes with deep convolutional neural network (DCNN) and segments single neurons by active contour with group shape similarity. We joint the segmentation and tracing together and they interact with each other by alternate iteration that tracing aids the selection of candidate region patch for active contour segmentation while the segmentation provides the neuron geometrical features which improve the robustness of tracing. The tracing model mainly relies on the neuron geometrical features and is updated after neuron being segmented on the every next section. Our method enables the reconstruction of neurons of the drosophila mushroom body which is cut to serial sections and imaged under SEM. Our method provides an elementary step for the whole reconstruction of neuronal networks.

  9. Inorganic trace analysis by mass spectrometry

    NASA Astrophysics Data System (ADS)

    Becker, Johanna Sabine; Dietze, Hans-Joachim

    1998-10-01

    Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g -1 concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of

  10. Determination of mineral, trace element, and pesticide levels in honey samples originating from different regions of Malaysia compared to manuka honey.

    PubMed

    Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

    2014-01-01

    The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination.

  11. Sex Difference in Draft-Legal Ultra-Distance Events - A Comparison between Ultra-Swimming and Ultra-Cycling.

    PubMed

    Salihu, Lejla; Rüst, Christoph Alexander; Rosemann, Thomas; Knechtle, Beat

    2016-04-30

    Recent studies reported that the sex difference in performance in ultra-endurance sports such as swimming and cycling changed over the years. However, the aspect of drafting in draft-legal ultra-endurance races has not yet been investigated. This study investigates the sex difference in ultra-swimming and ultra-cycling draft-legal races where drafting - swimming or cycling behind other participants to save energy and have more power at the end of the race to overtake them, is allowed. The change in performance of the annual best and the annual three best in an ultra-endurance swimming race (16-km 'Faros Swim Marathon') over 38 years and in a 24-h ultra-cycling race ('World Cycling Race') over 13 years were compared and analysed with respect to sex difference. Furthermore, performances of the fastest female and male finishers ever were compared. In the swimming event, the sex difference of the annual best male and female decreased non-significantly (P = 0.262) from 5.3% (1976) to 1.0% (2013). The sex gap of speed in the annual three fastest swimmers decreased significantly (P = 0.043) from 5.9 ± 1.6% (1979) to 4.7 ± 3.1% (2013). In the cycling event, the difference in cycling speed between the annual best male and female decreased significantly (P = 0.026) from 33.31% (1999) to 10.89% (2011). The sex gap of speed in the annual three fastest decreased significantly (P = 0.001) from 32.9 ± 0.6% (1999) to 16.4 ± 5.9% (2011). The fastest male swimmer ever (swimming speed 5.3 km/h, race time: 03:01:55 h:min:s) was 1.5% faster than the fastest female swimmer (swimming speed 5.2 km/h, race time: 03:04:09 h:min:s). The three fastest male swimmers ever (mean 5.27 ± 0.13 km/h) were 4.4% faster than the three fastest female swimmers (mean 5.05 ± 0.20 km/h) (P < 0.05). In the cycling event, the best male ever (cycling speed 45.8 km/h) was 26.4% faster than the best female (cycling speed 36.1 km/h). The three fastest male cyclists ever (45.9 km/h) (mean 45.85 ± 0.05 km

  12. The determination of trace elements in crude oil and its heavy fractions by atomic spectrometry

    NASA Astrophysics Data System (ADS)

    Duyck, Christiane; Miekeley, Norbert; Porto da Silveira, Carmem L.; Aucélio, Ricardo Q.; Campos, Reinaldo C.; Grinberg, Patrícia; Brandão, Geisamanda P.

    2007-09-01

    A literature review on the determination of trace elements in crude oil and heavy molecular mass fractions (saturates, aromatics, resins and asphaltenes) by ICP-MS, ICP OES and AAS is presented. Metal occurrences, forms and distributions are examined as well as their implications in terms of reservoir geochemistry, oil refining and environment. The particular analytical challenges for the determination of metals in these complex matrices by spectrochemical techniques are discussed. Sample preparation based on ashing, microwave-assisted digestion and combustion decomposition procedures is noted as robust and long used. However, the introduction of non-aqueous solvents and micro-emulsions into inductively coupled plasmas is cited as a new trend for achieving rapid and accurate analysis. Separation procedures for operationally defined fractions in crude oil are more systematically applied for the observation of metal distributions and their implications. Chemical speciation is of growing interest, achieved by the coupling of high efficiency separation techniques (e.g., HPLC and GC) to ICP-MS instrumentation, which allows the simultaneous determination of multiple organometallic species of geochemical and environmental importance.

  13. TRACE ELEMENT ANALYSES OF URANIUM MATERIALS

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

    Beals, D; Charles Shick, C

    The Savannah River National Laboratory (SRNL) has developed an analytical method to measure many trace elements in a variety of uranium materials at the high part-per-billion (ppb) to low part-per-million (ppm) levels using matrix removal and analysis by quadrapole ICP-MS. Over 35 elements were measured in uranium oxides, acetate, ore and metal. Replicate analyses of samples did provide precise results however none of the materials was certified for trace element content thus no measure of the accuracy could be made. The DOE New Brunswick Laboratory (NBL) does provide a Certified Reference Material (CRM) that has provisional values for a seriesmore » of trace elements. The NBL CRM were purchased and analyzed to determine the accuracy of the method for the analysis of trace elements in uranium oxide. These results are presented and discussed in the following paper.« less

  14. Outcome Assessments of Patients with Posttraumatic “Ultra-Time Vascular Injuries” of the Extremities

    PubMed Central

    Sun, Yi-Feng; Fang, Qiong-Xuan; Zhan, Hong-Yan; Wang, Fan; Cao, Wei; Zhao, Gang

    2015-01-01

    The management of posttraumatic vascular injury that presents after 8 h, or “ultra-time vascular injury”, is daunting, and inciting recognition of this injury is vital. We retrospectively analyzed 29 patients with ultra-time vascular injuries to determine the patients’ demographic characteristics and identify the determinants for amputation and disability. The age distribution of the high-risk population was from 18 years to 40 years, which indicated that these patients had plenty of productive life remaining. Injuries to the lower limbs (79.31%) were over four times more common than injuries to the upper limbs (17.24%), and open and blunt injuries occurred most commonly. The overall rate of limb salvage was 82.76% (24/29) and limb function is excellent in 45.83% (11/24) of the patients. The remaining patients experienced different degrees of disability in their limbs, which was determined by the anatomic location of the injury, and the presence of a combined arterial and venous injury, nerve injury, and complex soft tissue injury, as well as the occurrence of compartment syndrome. Hence, we recommend limb-salvage treatment for patients with traumatic ultra-time vascular injuries, particularly for those aged between 18 years and 40 years. Furthermore, we encourage the development of limb-salvage techniques for ultra-time vascular injuries. PMID:26639214

  15. Experimental determination of trace-element partitioning between pargasite and a synthetic hydrous andesitic melt

    NASA Astrophysics Data System (ADS)

    Brenan, J. M.; Shaw, H. F.; Ryerson, F. J.; Phinney, D. L.

    1995-10-01

    In order to more fully establish a basis for quantifying the role of amphibole in trace-element fractionation processes, we have measured pargasite/silicate melt partitioning of a variety of trace elements (Rb, Ba, Nb, Ta, Hf, Zr, Ce, Nd, Sm, Yb), including the first published values for U, Th and Pb. Experiments conducted at 1000°C and 1.5 GPa yielded large crystals free of compositional zoning. Partition coefficients were found to be constant at total concentrations ranging from ˜ 1 to > 100 ppm, indicating Henry's Law is oparative over this interval. Comparison of partition coefficients measured in this study with previous determinations yields good agreement for similar compositions at comparable pressure and temperature. The compatibility of U, Th and Pb in amphibole decreases in the order Pb > Th > U. Partial melting or fractional crystallization of amphibole-bearing assemblages will therefore result in the generation of excesses in 238U activity relative to 230Th, similar in magnitude to that produced by clinopyroxene. The compatibility of Pb in amphibole relative to U or Th indicates that melt generation in the presence of residual amphibole will result in the long-term enrichment in Pb relative to U or Th in the residue. This process is therefore incapable of producing the depletion in Pb relative to U or Th inferred from the Pb isotopic composition of MORB and OIB. Comparison of partition coefficients measured in this study with previous values for clinopyroxene allows some distinction to be made between expected trace-element fractionations produced during dry (cpx present) and wet (cpx + amphibole present) melting. Rb, Ba, Nb and Ta are dramatically less compatible in clinopyroxene than in amphibole, whereas Th, U, Hf and Zr have similar compatibilities in both phases. Interelement fractionations, such as DNb/DBa are also different for clinopyroxene and amphibole. Changes in certain ratios, such as Ba/Nb, Ba/Th, and Nb/Th within comagmatic suites may

  16. Practical applications of trace minerals for dairy cattle.

    PubMed

    Overton, T R; Yasui, T

    2014-02-01

    Trace minerals have critical roles in the key interrelated systems of immune function, oxidative metabolism, and energy metabolism in ruminants. To date, the primary trace elements of interest in diets for dairy cattle have included Zn, Cu, Mn, and Se although data also support potentially important roles of Cr, Co, and Fe in diets. Trace minerals such as Zn, Cu, Mn, and Se are essential with classically defined roles as components of key antioxidant enzymes and proteins. Available evidence indicates that these trace minerals can modulate aspects of oxidative metabolism and immune function in dairy cattle, particularly during the transition period and early lactation. Chromium has been shown to influence both immune function and energy metabolism of cattle; dairy cows fed Cr during the transition period and early lactation have evidence of improved immune function, increased milk production, and decreased cytological endometritis. Factors that complicate trace mineral nutrition at the farm level include the existence of a large number of antagonisms affecting bioavailability of individual trace minerals and uncertainty in terms of requirements under all physiological and management conditions; therefore, determining the optimum level and source of trace minerals under each specific situation continues to be a challenge. Typical factorial approaches to determine requirements for dairy cattle do not account for nuances in biological function observed with supplementation with various forms and amounts of trace minerals. Trace mineral nutrition modulates production, health, and reproduction in cattle although both formal meta-analysis and informal survey of the literature reveal substantial heterogeneity of response in these outcome variables. The industry has largely moved away from oxide-based programs toward sulfate-based programs; however, some evidence favors shifting supplementation strategies further toward more bioavailable forms of inorganic and organic trace

  17. Trace Element Analysis of Biological Samples.

    ERIC Educational Resources Information Center

    Veillon, Claude

    1986-01-01

    Reviews background of atomic absorption spectrometry techniques. Discusses problems encountered and precautions to be taken in determining trace elements in the parts-per-billion concentration range and below. Concentrates on determining chromium in biological samples by graphite furnace atomic absorption. Considers other elements, matrices, and…

  18. Rapid extraction and determination of 25 bioactive constituents in Alpinia oxyphylla using microwave extraction with ultra high performance liquid chromatography with tandem mass spectrometry.

    PubMed

    Sun, Zhi; Kong, Xiangzhen; Zuo, Lihua; Kang, Jian; Hou, Lei; Zhang, Xiaojian

    2016-02-01

    A novel and rapid microwave extraction and ultra high performance liquid chromatography with tandem mass spectrometry method was developed and validated for the simultaneous determination of 25 bioactive constituents (including two new constituents) in Fructus Alpinia oxyphylla. The optimized conditions of the microwave extraction was a microwave power of 300 W, extraction temperature of 80°C, solvent-to-solid ratio of 30 mL/g and extraction time of 8 min. Separation was achieved on a Waters ACQUITY UPLC(®) HSS C18 column (2.1 mm× 50 mm, 1.8 μm) using gradient elution with a mobile phase consisting of acetonitrile and 1 mM ammonium acetate at a flow rate of 0.2 mL/min. This is the first report of the simultaneous determination of 25 bioactive constituents in Fructus Alpinia oxyphylla by ultra high performance liquid chromatography with tandem mass spectrometry. The method was validated with good linearity, acceptable precision and accuracy. The validated method was successfully applied to determine the contents of 25 bioactive constituents in Fructus Alpinia oxyphylla from different sources and the analysis results were classified by hierarchical cluster analysis, which indicated the effect of different cultivation regions on the contents of constituents. This study provides powerful and practical guidance in the quality control of Alpinia oxyphylla and lays the foundation for further research of Alpinia oxyphylla. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Ambient methods and apparatus for rapid laser trace constituent analysis

    DOEpatents

    Snyder, Stuart C.; Partin, Judy K.; Grandy, Jon D.; Jeffery, Charles L.

    2002-01-01

    A method and apparatus are disclosed for measuring trace amounts of constituents in samples by using laser induced breakdown spectroscopy and laser induced fluorescence under ambient conditions. The laser induced fluorescence is performed at a selected wavelength corresponding to an absorption state of a selected trace constituent. The intensity value of the emission decay signal which is generated by the trace constituent is compared to calibrated emission intensity decay values to determine the amount of trace constituent present.

  20. Effects of Dissociation/Recombination on the Day–Night Temperature Contrasts of Ultra-hot Jupiters

    NASA Astrophysics Data System (ADS)

    Komacek, Thaddeus D.; Tan, Xianyu

    2018-05-01

    Secondary eclipse observations of ultra-hot Jupiters have found evidence that hydrogen is dissociated on their daysides. Additionally, full-phase light curve observations of ultra-hot Jupiters show a smaller day-night emitted flux contrast than that expected from previous theory. Recently, it was proposed by Bell & Cowan (2018) that the heat intake to dissociate hydrogen and heat release due to recombination of dissociated hydrogen can affect the atmospheric circulation of ultra-hot Jupiters. In this work, we add cooling/heating due to dissociation/recombination into the analytic theory of Komacek & Showman (2016) and Zhang & Showman (2017) for the dayside-nightside temperature contrasts of hot Jupiters. We find that at high values of incident stellar flux, the day-night temperature contrast of ultra-hot Jupiters may decrease with increasing incident stellar flux due to dissociation/recombination, the opposite of that expected without including the effects of dissociation/recombination. We propose that a combination of a greater number of full-phase light curve observations of ultra-hot Jupiters and future General Circulation Models that include the effects of dissociation/recombination could determine in detail how the atmospheric circulation of ultra-hot Jupiters differs from that of cooler planets.

  1. Indirect spectrophotometric determination of ultra trace amounts of selenium based on dispersive liquid-liquid microextraction-solidified floating organic drop.

    PubMed

    Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Nozohor, Mahnaz

    2013-12-01

    A novel dispersive liquid-liquid microextraction-solidified floating organic drop (DLLME-SFOD) method combined with fiber optic-linear array detection spectrophotometry has been developed for the indirect determination of selenium. The method is based on the oxidation of the I(-) to iodine by inorganic Se(IV). The produced I2 reacts with the excess of I(-) ions in acidic media to give triiodide ions. The I3(-) is then extracted into 1-undecanol by DLLME-SFOD upon the formation of an ion pair with cetyltrimethylammonium cation. The extracted ion pair is determined by measuring its absorption at 360 nm. The absorbance signal is proportional to the selenium concentration in the aqueous phase. Under optimum conditions, the method provided an enrichment factor of 250 with a detection limit of 16.0 μg L(-1) and a linear dynamic range of 40.0-1000.0 μg L(-1). The relative standard deviation was found to be 2.1% (n=7) at 100.0 μg L(-1) concentration level. The method was successfully applied to th e determination of selenium in water samples and selenium plus tablet. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. [Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Lech, Rodziewicz; Jolanta, MasŁOwiecka; Anna, Sadowska; Halina, Car

    2017-10-08

    Five thyreostats (TSs), namely tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil, were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in positive electrospray ionization mode. Extraction and clean-up were achieved using a ChemElut cartridge with tert -butyl methyl ether, without a derivatization step. Separation was achieved on an Acquity UPLC SS T3 column. The mobile phase was acetonitrile and water containing 0.2% (v/v) formic acid. The mass spectrometer was operated in multiple reaction monitoring mode. Urine samples were spiked with TS solution at levels corresponding to 5, 10, 15, and 20 μg/L. The accuracy (internal standard corrected) ranged from 92% to 107%, with a repeatability precision (relative standard deviation, RSD) less than 15% for all five analytes. The RSDs within-laboratory reproducibility was less than 26%. The decision limits (CCα) and detection capabilities (CCβ) were obtained from a calibration curve and were in the ranges of 3.1-6.1 μg/L and 4.0-7.4 μg/L, respectively. The CCα and CCβ values were below the recommended concentration, which was set at 10 μg/L. The results show that the described method is suitable for the direct detection of TSs in bovine urine. This method can also be used to determine TSs in porcine urine.

  3. Determination of endocrine disrupting chemicals and antiretroviral compounds in surface water: A disposable sorptive sampler with comprehensive gas chromatography - Time-of-flight mass spectrometry and large volume injection with ultra-high performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Wooding, Madelien; Rohwer, Egmont R; Naudé, Yvette

    2017-05-05

    Many rural dwellers and inhabitants of informal settlements in South Africa are without access to treated water and collect untreated water from rivers and dams for personal use. Endocrine disrupting chemicals (EDCs) have been detected in surface water and wildlife of South Africa. EDCs are often present in complex environmental matrices at ultra-trace levels complicating detection thereof. We report a simplified multi-residue approach for the detection and quantification of EDCs, emerging EDCs, and antiretroviral drugs in surface water. A low cost (less than one US dollar), disposable, sorptive extraction sampler was prepared in-house. The disposable samplers consisted of polydimethylsiloxane (PDMS) tubing fashioned into a loop which was then placed in water samples to concentrate EDCs and emerging pollutants. The PDMS samplers were thermally desorbed directly in the inlet of a GC, thereby eliminating the need for expensive consumable cryogenics. Comprehensive gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOFMS) was used for compound separation and identification. Linear retention indices of EDCs and emerging pollutants were determined on a proprietary Crossbond ® phase Rtx ® -CLPesticides II GC capillary column. In addition, large volume injection of surface water into an ultra-performance liquid chromatograph tandem mass spectrometer (UPLC-MS/MS) was used as complementary methodology for the detection of less volatile compounds. Large volume injection reduced tedious and costly sample preparation steps. Limits of detection for the GC method ranged from 1 to 98pg/l and for the LC method from 2 to 135ng/l. Known and emerging EDCs such as pharmaceuticals, personal care products and pesticides, as well as the antiretroviral compounds, efavirenz and nevirapine, were detected in surface water from South Africa at concentration levels ranging from 0.16ng/l to 227ng/l. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Kinetic spectrophotometric method for trace determination of thiocyanate based on its inhibitory effect

    NASA Astrophysics Data System (ADS)

    Naik, Radhey M.; Kumar, Basant; Asthana, Abhas

    2010-03-01

    A kinetic spectrophotometric method for the determination of thiocyanate, based on its inhibitory effect on silver(I) catalyzed substitution of cyanide ion, by phenylhydrazine in hexacyanoferrate(II) is described. Thiocyanate ions form strong complexes with silver(I) catalyst which is used as the basis for its determination at trace level. The progress of reaction was monitored, spectrophotometrically, at 488 nm ( λmax of [Fe(CN) 5PhNHNH 2] 3-, complex) under the optimum reaction conditions at: 2.5 × 10 -3 M [Fe(CN) 6] 4-, 1.0 × 10 -3 M [PhNHNH 2], 8.0 × 10 -7 M [Ag +], pH 2.8 ± 0.02, ionic strength ( μ) 0.02 M (KNO 3) and temperature 30 ± 0.1 °C. A linear relationship obtained between absorbance (measured at 488 nm at different times) and inhibitor concentration, under specified conditions, has been used for the determination of [thiocyanate] in the range of 0.8-8.0 × 10 -8 M with a detection limit of 2 × 10 -9 M. The standard deviation and percentage error have been calculated and reported with each datum. A most plausible mechanistic scheme has been proposed for the reaction. The values of equilibrium constants for complex formation between catalyst-inhibitor ( KCI), catalyst-substrate ( Ks) and Michaelis-Menten constant ( Km) have been computed from the kinetic data. The influence of possible interference by major cations and anions on the determination of thiocyanate and their limits has been investigated.

  5. Ultra-Large Solar Sail

    NASA Technical Reports Server (NTRS)

    Burton, Rodney; Coverstone, Victoria

    2009-01-01

    UltraSail is a next-generation ultra-large (km2 class) sail system. Analysis of the launch, deployment, stabilization, and control of these sails shows that high-payload-mass fractions for interplanetary and deep-space missions are possible. UltraSail combines propulsion and control systems developed for formation-flying microsatellites with a solar sail architecture to achieve controllable sail areas approaching 1 km2. Electrically conductive CP-1 polyimide film results in sail subsystem area densities as low as 5 g/m2. UltraSail produces thrust levels many times those of ion thrusters used for comparable deep-space missions. The primary innovation involves the near-elimination of sail-supporting structures by attaching each blade tip to a formation- flying microsatellite, which deploys the sail and then articulates the sail to provide attitude control, including spin stabilization and precession of the spin axis. These microsatellite tips are controlled by microthrusters for sail-film deployment and mission operations. UltraSail also avoids the problems inherent in folded sail film, namely stressing, yielding, or perforating, by storing the film in a roll for launch and deployment. A 5-km long by 2 micrometer thick film roll on a mandrel with a 1 m circumference (32 cm diameter) has a stored thickness of 5 cm. A 5 m-long mandrel can store a film area of 25,000 m2, and a four-blade system has an area of 0.1 sq km.

  6. Visualizing an ultra-weak protein-protein interaction in phosphorylation signaling.

    PubMed

    Xing, Qiong; Huang, Peng; Yang, Ju; Sun, Jian-Qiang; Gong, Zhou; Dong, Xu; Guo, Da-Chuan; Chen, Shao-Min; Yang, Yu-Hong; Wang, Yan; Yang, Ming-Hui; Yi, Ming; Ding, Yi-Ming; Liu, Mai-Li; Zhang, Wei-Ping; Tang, Chun

    2014-10-20

    Proteins interact with each other to fulfill their functions. The importance of weak protein-protein interactions has been increasingly recognized. However, owing to technical difficulties, ultra-weak interactions remain to be characterized. Phosphorylation can take place via a K(D)≈25 mM interaction between two bacterial enzymes. Using paramagnetic NMR spectroscopy and with the introduction of a novel Gd(III)-based probe, we determined the structure of the resulting complex to atomic resolution. The structure accounts for the mechanism of phosphoryl transfer between the two enzymes and demonstrates the physical basis for their ultra-weak interaction. Further, molecular dynamics (MD) simulations suggest that the complex has a lifetime in the micro- to millisecond regimen. Hence such interaction is termed a fleeting interaction. From mathematical modeling, we propose that an ultra-weak fleeting interaction enables rapid flux of phosphoryl signal, providing a high effective protein concentration. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. 76 FR 29765 - Determination of System Attributes for the Tracking and Tracing of Prescription Drugs; Reopening...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-05-23

    ... a track-and-trace system and for obtaining input from supply chain partners on potential attributes...-trace system and (2) input from supply chain partners on potential attributes and standards for the...

  8. On the Nature of Ultra-faint Dwarf Galaxy Candidates. II. The Case of Cetus II

    NASA Astrophysics Data System (ADS)

    Conn, Blair C.; Jerjen, Helmut; Kim, Dongwon; Schirmer, Mischa

    2018-04-01

    We obtained deep Gemini GMOS-S g, r photometry of the ultra-faint dwarf galaxy candidate Cetus II with the aim of providing stronger constraints on its size, luminosity, and stellar population. Cetus II is an important object in the size–luminosity plane, as it occupies the transition zone between dwarf galaxies and star clusters. All known objects smaller than Cetus II (r h ∼ 20 pc) are reported to be star clusters, while most larger objects are likely dwarf galaxies. We found a prominent excess of main-sequence stars in the color–magnitude diagram of Cetus II, best described by a single stellar population with an age of 11.2 Gyr, metallicity of [Fe/H] = ‑1.28 dex, an [α/Fe] = 0.0 dex at a heliocentric distance of 26.3 ± 1.2 kpc. As well as being spatially located within the Sagittarius dwarf tidal stream, these properties are well matched to the Sagittarius galaxy’s Population B stars. Interestingly, like our recent findings on the ultra-faint dwarf galaxy candidate Tucana V, the stellar field in the direction of Cetus II shows no evidence of a concentrated overdensity despite tracing the main sequence for over six magnitudes. These results strongly support the picture that Cetus II is not an ultra-faint stellar system in the Milky Way halo, but made up of stars from the Sagittarius tidal stream.

  9. Trace analysis of high-purity graphite by LA-ICP-MS.

    PubMed

    Pickhardt, C; Becker, J S

    2001-07-01

    Laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been established as a very efficient and sensitive technique for the direct analysis of solids. In this work the capability of LA-ICP-MS was investigated for determination of trace elements in high-purity graphite. Synthetic laboratory standards with a graphite matrix were prepared for the purpose of quantifying the analytical results. Doped trace elements, concentration 0.5 microg g(-1), in a laboratory standard were determined with an accuracy of 1% to +/- 7% and a relative standard deviation (RSD) of 2-13%. Solution-based calibration was also used for quantitative analysis of high-purity graphite. It was found that such calibration led to analytical results for trace-element determination in graphite with accuracy similar to that obtained by use of synthetic laboratory standards for quantification of analytical results. Results from quantitative determination of trace impurities in a real reactor-graphite sample, using both quantification approaches, were in good agreement. Detection limits for all elements of interest were determined in the low ng g(-1) concentration range. Improvement of detection limits by a factor of 10 was achieved for analyses of high-purity graphite with LA-ICP-MS under wet plasma conditions, because the lower background signal and increased element sensitivity.

  10. Parametric Trace Slicing

    NASA Technical Reports Server (NTRS)

    Rosu, Grigore (Inventor); Chen, Feng (Inventor); Chen, Guo-fang; Wu, Yamei; Meredith, Patrick O. (Inventor)

    2014-01-01

    A program trace is obtained and events of the program trace are traversed. For each event identified in traversing the program trace, a trace slice of which the identified event is a part is identified based on the parameter instance of the identified event. For each trace slice of which the identified event is a part, the identified event is added to an end of a record of the trace slice. These parametric trace slices can be used in a variety of different manners, such as for monitoring, mining, and predicting.

  11. Determination of Mineral, Trace Element, and Pesticide Levels in Honey Samples Originating from Different Regions of Malaysia Compared to Manuka Honey

    PubMed Central

    Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

    2014-01-01

    The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination. PMID:24982869

  12. A general, cryogenically-based analytical technique for the determination of trace quantities of volatile organic compounds in the atmosphere

    NASA Technical Reports Server (NTRS)

    Coleman, R. A.; Cofer, W. R., III; Edahl, R. A., Jr.

    1985-01-01

    An analytical technique for the determination of trace (sub-ppbv) quantities of volatile organic compounds in air was developed. A liquid nitrogen-cooled trap operated at reduced pressures in series with a Dupont Nafion-based drying tube and a gas chromatograph was utilized. The technique is capable of analyzing a variety of organic compounds, from simple alkanes to alcohols, while offering a high level of precision, peak sharpness, and sensitivity.

  13. Determining trace gas efflux from container production of woody nursery crops

    USDA-ARS?s Scientific Manuscript database

    In recent years, climate change and its effects on the global environment has garnered significant attention from the scientific community. Increased trace gas emissions of carbon dioxide (CO2), methane (CH4) and nitrous oxide (N2O) are widely believed to be the driving force behind global warming. ...

  14. 77 FR 59182 - Ultra-Deepwater Advisory Committee

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-09-26

    ... DEPARTMENT OF ENERGY Ultra-Deepwater Advisory Committee AGENCY: Office of Fossil Energy... of the Ultra-Deepwater Advisory Committee is to provide advice on development and implementation of programs related to ultra-deepwater architecture and technology to the Secretary of Energy and provide...

  15. Quality control of modified xiaoyao san through the determination of 22 active components by ultra-performance liquid chromatography.

    PubMed

    Qin, Feng; Huang, Jun; Qiu, Xinjian; Hu, Sihang; Huang, Xi

    2011-01-01

    A simple, sensitive, and reliable ultra-performance liquid chromatography (UPLC) method has been developed for simultaneous determination of 22 major constituents in modified xiaoyao san (MXS), a multiherbal formula. The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column (150 x 2.1 mm, 1.7 microm, particle size), with an aqueous 0.5% acetic acid and acetonitrile mobile phase gradient. The method was validated for linearity (r2 >0.9937), intraday and interday precision (RSD <8.51%), recovery (91.18-107.73%), LOD (0.02-4.17 ng/mL), and LOQ (0.05-12.50 ng/mL). The established method was successfully applied to quantify the 22 marker compounds in MXS, which provided a useful basis of overall evaluation of the quality of MXS.

  16. Determination of trace elements in the reproduction systems of some rare animals using pixe

    NASA Astrophysics Data System (ADS)

    Suqing, Chen; Nengming, Wang; Jianxuan, Chen; Dazhong, Zhang

    In order to search for the significance of artificial feeding, reproduction and heredity, trace elements in the reproductive systems of some rare animals, including giant panda, lesser panda, marmot and river deer, have been determined. Typcial X-ray spectra of various samples are given. The elemental contents in ovary and testis of the giant panda and the lesser panda are calculated by means of yttrium as an internal standard. Elemental relative concentrations are calculated from peak areas in the spectra for thick samples. It is found that for the concentration of the elements Cr, Mn, Fe, Ni, Cu, As in the ovary there exist no significant different between the giant panda and the lesser panda. The concentration of Zn, however, shows a remakable difference. The importance of zinc in biological processes is discussed.

  17. Points to consider: efficacy and safety evaluations in the clinical development of ultra-orphan drugs.

    PubMed

    Maeda, Kojiro; Kaneko, Masayuki; Narukawa, Mamoru; Arato, Teruyo

    2017-08-23

    The unmet medical needs of individuals with very rare diseases are high. The clinical trial designs and evaluation methods used for 'regular' drugs are not applicable in the clinical development of ultra-orphan drugs (<1000 patients) in many cases. In order to improve the clinical development of ultra-orphan drugs, we examined several points regarding the efficient evaluations of drug efficacy and safety that could be conducted even with very small sample sizes, based on the review reports of orphan drugs approved in Japan. The clinical data packages of 43 ultra-orphan drugs approved in Japan from January 2001 to December 2014 were investigated. Japanese clinical trial data were not included in the clinical data package for eight ultra-orphan drugs, and non-Japanese clinical trial data were included for six of these eight drug. Japanese supportive data that included retrospective studies, published literature, clinical research and Japanese survey results were clinical data package attachments in 22 of the 43 ultra-orphan drugs. Multinational trials were conducted for three ultra-orphan drugs. More than two randomized controlled trials (RCTs) were conducted for only 11 of the 43 ultra-orphan drugs. The smaller the number of patients, the greater the proportion of forced titration and optional titration trials were conducted. Extension trials were carried out for enzyme preparations and monoclonal antibodies with high ratio. Post-marketing surveillance of all patients was required in 36 of the 43 ultra-orphan drugs. For ultra-orphan drugs, clinical endpoints were used as the primary efficacy endpoint of the pivotal trial only for two drugs. The control groups in RCTs were classified as follows: placebo groups different dosage groups, and active controls groups. Sample sizes have been determined on the basis of feasibility for some ultra-orphan drugs. We provide "Draft Guidance on the Clinical Development of Ultra-Orphan Drugs" based on this research. The development

  18. A method for trace element determination of single Daphnia specimens using total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Mages, Margarete; Woelfl, Stefan; v. Tümpling jun, Wolf

    2001-11-01

    Two new preparation techniques for total-reflection X-ray fluorescence (TXRF) element determination of single freshwater crustacean specimens (dry weight: 3-40 μg ind -1) have been developed and tested using Daphnia pulex from a deep, oligotrophic freshwater lake located in southern Chile. Dry method: Specimens were washed with 0.2 μm filtered lake water and frozen in liquid nitrogen. The freeze-dried Daphnia specimens were weighed using an ultra-fine microbalance and placed on quartz glass carriers for TXRF analysis. Wet method: Specimens were washed with 0.2 μm filtered lake water and placed on quartz glass carriers for TXRF analysis and dried in air. The dry weight was determined using the previously established body length-dry weight relationship. Method validation for both the dry and the wet preparation method in combination with TXRF spectrometry for the element determination in small single freshwater crustaceans showed that both methods can be used for routine investigations. There were no significant differences between the dry and the wet methods concerning the elements Ca, K, Fe, Zn, Br, P, Cu, but the determination of Mn, S and Sr revealed significant differences between the two methods. It seems that the dry method yields more precise results, but the wet method is easier to handle in the field when samples cannot be fixed with liquid nitrogen.

  19. Ultra Reliable Closed Loop Life Support for Long Space Missions

    NASA Technical Reports Server (NTRS)

    Jones, Harry W.; Ewert, Michael K.

    2010-01-01

    Spacecraft human life support systems can achieve ultra reliability by providing sufficient spares to replace all failed components. The additional mass of spares for ultra reliability is approximately equal to the original system mass, provided that the original system reliability is not too low. Acceptable reliability can be achieved for the Space Shuttle and Space Station by preventive maintenance and by replacing failed units. However, on-demand maintenance and repair requires a logistics supply chain in place to provide the needed spares. In contrast, a Mars or other long space mission must take along all the needed spares, since resupply is not possible. Long missions must achieve ultra reliability, a very low failure rate per hour, since they will take years rather than weeks and cannot be cut short if a failure occurs. Also, distant missions have a much higher mass launch cost per kilogram than near-Earth missions. Achieving ultra reliable spacecraft life support systems with acceptable mass will require a well-planned and extensive development effort. Analysis must determine the reliability requirement and allocate it to subsystems and components. Ultra reliability requires reducing the intrinsic failure causes, providing spares to replace failed components and having "graceful" failure modes. Technologies, components, and materials must be selected and designed for high reliability. Long duration testing is needed to confirm very low failure rates. Systems design should segregate the failure causes in the smallest, most easily replaceable parts. The system must be designed, developed, integrated, and tested with system reliability in mind. Maintenance and reparability of failed units must not add to the probability of failure. The overall system must be tested sufficiently to identify any design errors. A program to develop ultra reliable space life support systems with acceptable mass should start soon since it must be a long term effort.

  20. 75 FR 48319 - Ultra-Deepwater Advisory Committee

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-08-10

    ... DEPARTMENT OF ENERGY Ultra-Deepwater Advisory Committee AGENCY: Department of Energy, Office of...: Purpose of the Committee: The purpose of the Ultra-Deepwater Advisory Committee is to provide advice on development and implementation of programs related to ultra-deepwater architecture and technology to the...

  1. 76 FR 77990 - Ultra-Deepwater Advisory Committee

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-12-15

    ... DEPARTMENT OF ENERGY Ultra-Deepwater Advisory Committee AGENCY: Office of Fossil Energy... Committee: The purpose of the Ultra-Deepwater Advisory Committee is to provide advice to the Secretary of Energy on development and implementation of programs related to ultra-deepwater natural gas and other...

  2. 76 FR 6775 - Ultra-Deepwater Advisory Committee

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-02-08

    ... DEPARTMENT OF ENERGY Ultra-Deepwater Advisory Committee AGENCY: Department of Energy, Office of... Committee: The purpose of the Ultra-Deepwater Advisory Committee is to provide advice on development and implementation of programs related to ultra-deepwater architecture and technology to the Secretary of Energy and...

  3. 75 FR 54860 - Ultra Deepwater Advisory Committee

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-09-09

    ... DEPARTMENT OF ENERGY Ultra Deepwater Advisory Committee AGENCY: Department of Energy, Office of... of an open meeting of the Ultra Deepwater Advisory Committee. The Committee was organized pursuant to.../advisorycommittees/UltraDeepwater.html . Issued in Washington, DC, on September 3, 2010. Carol A. Matthews, Committee...

  4. Fast log P determination by ultra-high-pressure liquid chromatography coupled with UV and mass spectrometry detections.

    PubMed

    Henchoz, Yveline; Guillarme, Davy; Martel, Sophie; Rudaz, Serge; Veuthey, Jean-Luc; Carrupt, Pierre-Alain

    2009-08-01

    Ultra-high-pressure liquid chromatography (UHPLC) systems able to work with columns packed with sub-2 microm particles offer very fast methods to determine the lipophilicity of new chemical entities. The careful development of the most suitable experimental conditions presented here will help medicinal chemists for high-throughput screening (HTS) log P(oct) measurements. The approach was optimized using a well-balanced set of 38 model compounds and a series of 28 basic compounds such as beta-blockers, local anesthetics, piperazines, clonidine, and derivatives. Different organic modifiers and hybrid stationary phases packed with 1.7-microm particles were evaluated in isocratic as well as gradient modes, and the advantages and limitations of tested conditions pointed out. The UHPLC approach offered a significant enhancement over the classical HPLC methods, by a factor 50 in the lipophilicity determination throughput. The hyphenation of UHPLC with MS detection allowed a further increase in the throughput. Data and results reported herein prove that the UHPLC-MS method can represent a progress in the HTS-measurement of lipophilicity due to its speed (at least a factor of 500 with respect to HPLC approaches) and to an extended field of application.

  5. Determination of the 240Pu/ 239Pu atomic ratio in soils from Palomares (Spain) by low-energy accelerator mass spectrometry

    NASA Astrophysics Data System (ADS)

    Chamizo, E.; García-León, M.; Synal, H.-A.; Suter, M.; Wacker, L.

    2006-08-01

    In 1966, the nuclear fuel of two thermonuclear bombs was released over the Spanish region of Palomares, due to a B52 bomber accident during a refuelling operation. Since then, much effort has been made to assess its impact to the different environmental compartments of this area in South-East Spain, mostly by measuring the 239+240Pu activity concentration and the 238Pu/239+240Pu activity ratio. Nevertheless, these measurements do not give enough information on the problem. In order to recognize unambiguously small traces of the weapon-grade plutonium released in the accident, the ratio of the two major isotopes of plutonium, 240Pu/239Pu, has to be determined. In this work, this ratio has been measured in low- and high-activity samples from Palomares by means of low-energy accelerator mass spectrometry (AMS). That way, we will show the potential of the new generation of compact AMS facilities in terms of plutonium characterization at ultra-trace levels.

  6. [Determination of 12 flavonoids in tobacco leaves using ultra-high performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Li, Yong; Lin, Qian; Pang, Tao; Shi, Junli

    2015-07-01

    Flavonoids are very important secondary metabolites for tobacco plants. They are also considered as important flavor precursors for cigarettes. A method of ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established for the simultaneous determination of 12 flavonoids in tobacco leaves. The developed method determined 10 more flavonoids compared to the traditional method. A solution of methanol-water-chloroform (5:2:2, v/v/v) was used to extract the flavonoids from tobacco leaves and remove the pigment. Instrument analysis using the UPLC-MS/MS was completed in 13 min. The method validation was performed, and the results showed that the linear correlation coefficients (r2) of all the 12 flavonoids were more than 0.99. The limits of detection and the limits of quantification were in the range of 0.3-100 μg/L and 1.2-400 μg/L, respectively. Intra-day and Inter-day reproducibilities were in the range of 3.5%-7.4% and 5.2%-11.4%, respectively. The recoveries were 81.2%-111.9%. The established method was successfully used to analyze the flavonoids of tobacco leaves of 11 varieties. Significant concentration differences of the flavonoids were found among the determined varieties. Furthermore, significant positive correlation among the flavonoids with similar chemical structures (aglycones and their related glycosides, glycosides with the same aglycone, and similar aglycones) was found using the acquired data.

  7. Infrared trace element detection system

    DOEpatents

    Bien, Fritz; Bernstein, Lawrence S.; Matthew, Michael W.

    1988-01-01

    An infrared trace element detection system including an optical cell into which the sample fluid to be examined is introduced and removed. Also introduced into the optical cell is a sample beam of infrared radiation in a first wavelength band which is significantly absorbed by the trace element and a second wavelength band which is not significantly absorbed by the trace element for passage through the optical cell through the sample fluid. The output intensities of the sample beam of radiation are selectively detected in the first and second wavelength bands. The intensities of a reference beam of the radiation are similarly detected in the first and second wavelength bands. The sensed output intensity of the sample beam in one of the first and second wavelength bands is normalized with respect to the other and similarly, the intensity of the reference beam of radiation in one of the first and second wavelength bands is normalized with respect to the other. The normalized sample beam intensity and normalized reference beam intensity are then compared to provide a signal from which the amount of trace element in the sample fluid can be determined.

  8. Infrared trace element detection system

    DOEpatents

    Bien, F.; Bernstein, L.S.; Matthew, M.W.

    1988-11-15

    An infrared trace element detection system includes an optical cell into which the sample fluid to be examined is introduced and removed. Also introduced into the optical cell is a sample beam of infrared radiation in a first wavelength band which is significantly absorbed by the trace element and a second wavelength band which is not significantly absorbed by the trace element for passage through the optical cell through the sample fluid. The output intensities of the sample beam of radiation are selectively detected in the first and second wavelength bands. The intensities of a reference beam of the radiation are similarly detected in the first and second wavelength bands. The sensed output intensity of the sample beam in one of the first and second wavelength bands is normalized with respect to the other and similarly, the intensity of the reference beam of radiation in one of the first and second wavelength bands is normalized with respect to the other. The normalized sample beam intensity and normalized reference beam intensity are then compared to provide a signal from which the amount of trace element in the sample fluid can be determined. 11 figs.

  9. UltraNet Target Parameters. Chapter 1

    NASA Technical Reports Server (NTRS)

    Kislitzin, Katherine T.; Blaylock, Bruce T. (Technical Monitor)

    1992-01-01

    The UltraNet is a high speed network capable of rates up to one gigabit per second. It is a hub based network with four optical fiber links connecting each hub. Each link can carry up to 256 megabits of data, and the hub backplane is capable of one gigabit aggregate throughput. Host connections to the hub may be fiber, coax, or channel based. Bus based machines have adapter boards that connect to transceivers in the hub, while channel based machines use a personality module in the hub. One way that the UltraNet achieves its high transfer rates is by off-loading the protocol processing from the hosts to special purpose protocol engines in the UltraNet hubs. In addition, every hub has a PC connected to it by StarLAN for network management purposes. Although there is hub resident and PC resident UltraNet software, this document treats only the host resident UltraNet software.

  10. Ultra-wideband radar motion sensor

    DOEpatents

    McEwan, Thomas E.

    1994-01-01

    A motion sensor is based on ultra-wideband (UWB) radar. UWB radar range is determined by a pulse-echo interval. For motion detection, the sensors operate by staring at a fixed range and then sensing any change in the averaged radar reflectivity at that range. A sampling gate is opened at a fixed delay after the emission of a transmit pulse. The resultant sampling gate output is averaged over repeated pulses. Changes in the averaged sampling gate output represent changes in the radar reflectivity at a particular range, and thus motion.

  11. Ultra-wideband radar motion sensor

    DOEpatents

    McEwan, T.E.

    1994-11-01

    A motion sensor is based on ultra-wideband (UWB) radar. UWB radar range is determined by a pulse-echo interval. For motion detection, the sensors operate by staring at a fixed range and then sensing any change in the averaged radar reflectivity at that range. A sampling gate is opened at a fixed delay after the emission of a transmit pulse. The resultant sampling gate output is averaged over repeated pulses. Changes in the averaged sampling gate output represent changes in the radar reflectivity at a particular range, and thus motion. 15 figs.

  12. Determination of seven bisphenol analogues in reed and Callitrichaceae by ultra performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Lu, Libin; Yang, Yunjia; Zhang, Jing; Shao, Bing

    2014-03-15

    An analytical procedure was developed to simultaneously determine bisphenol S, bisphenol F, bisphenol B, bisphenol A, bisphenol AF, tetrachlorobisphenol A, and tetrabromobisphenol A in reed and Callitrichaceae. Homogenized samples were extracted with acetonitrile and purified using an ENVI™-Carb cartridge followed by an NH2 cartridge. The analytes were separated and quantified by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The recoveries at three fortified levels in reed and Callitrichaceae were 57-108% and 68-106%, respectively, with relative standard deviations of no more than 15% (n=6). The method limits of quantification and detection for the seven bisphenol analogues were 0.005-0.500μg/kg and 0.002-0.150μg/kg, respectively. This method was used to analyze the seven compounds in ten reed and Callitrichaceae samples collected from Zhejiang, China. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Determination of trace rare earth elements in gadolinium aluminate by inductively coupled plasma time of flight mass spectrometry

    NASA Astrophysics Data System (ADS)

    Saha, Abhijit; Deb, S. B.; Nagar, B. K.; Saxena, M. K.

    An analytical methodology was developed for the precise quantification of ten trace rare earth elements (REEs), namely, La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, and Tm, in gadolinium aluminate (GdAlO3) employing an ultrasonic nebulizer (USN)-desolvating device based inductively coupled plasma mass spectrometry (ICP-MS). A microwave digestion procedure was optimized for digesting 100 mg of the refractory oxide using a mixture of sulphuric acid (H2SO4), phosphoric acid (H3PO4) and water (H2O) with 1400 W power, 10 min ramp and 60 min hold time. An USN-desolvating sample introduction system was employed to enhance analyte sensitivities by minimizing their oxide ion formation in the plasma. Studies on the effect of various matrix concentrations on the analyte intensities revealed that precise quantification of the analytes was possible with matrix level of 250 mg L- 1. The possibility of using indium as an internal standard was explored and applied to correct for matrix effect and variation in analyte sensitivity under plasma operating conditions. Individual oxide ion formation yields were determined in matrix matched solution and employed for correcting polyatomic interferences of light REE (LREE) oxide ions on the intensities of middle and heavy rare earth elements (MREEs and HREEs). Recoveries of ≥ 90% were achieved for the analytes employing standard addition technique. Three real samples were analyzed for traces of REEs by the proposed method and cross validated for Eu and Nd by isotope dilution mass spectrometry (IDMS). The results show no significant difference in the values at 95% confidence level. The expanded uncertainty (coverage factor 1σ) in the determination of trace REEs in the samples were found to be between 3 and 8%. The instrument detection limits (IDLs) and the method detection limits (MDLs) for the ten REEs lie in the ranges 1-5 ng L- 1 and 7-64 μg kg- 1 respectively.

  14. Determination of trace elements in metals and alloys by atomic-absorption spectroscopy using an induction-heated graphite well furnace as atom source.

    PubMed

    Headridge, J B; Smith, D R

    1972-07-01

    An induction-heated graphite furnace, coupled to a Unicam SP 90 atomic-absorption spectrometer, is described for the direct determination of trace elements in metals and alloys. The furnace is capable of operation at temperatures up to 2400 degrees , and has been used to obtain calibration graphs for the determination of ppm quantities of bismuth in lead-base alloys, cast irons and stainless steels, and for the determination of cadmium at the ppm level in zinc-base alloys. Milligram samples of the alloys were atomized directly. Calibration graphs for the determination of the elements in solutions were obtained for comparison. The accuracy and precision of the determination are presented and discussed.

  15. Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

    PubMed

    Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

    2016-05-01

    Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples.

  16. 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

  17. Graphene-based solid-phase extraction disk for fast separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples.

    PubMed

    Wang, Zonghua; Han, Qiang; Xia, Jianfei; Xia, Linhua; Ding, Mingyu; Tang, Jie

    2013-06-01

    Graphene has great potentials for the use in sample preparation due to its ultra high specific surface area, superior chemical stability, and excellent thermal stability. In our work, a novel graphene-based SPE disk was developed for separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples. Based on the strong π-π stacking interaction between the analytes and graphene, the analytes extracted by graphene were eluted by cyclohexane and then determined by GC-MS. Under the optimized conditions, high flow rate (30 mL/min) and sensitivity (0.84-13 ng/L) were achieved. The proposed method was successfully applied to the analysis of real environmental water samples with recoveries ranging from 72.8 to 106.2%. Furthermore, the property of anticlogging and reusability was also improved. This work reveals great potentials of graphene-based SPE disk in environmental analytical. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Ultra-stripped supernovae: progenitors and fate

    NASA Astrophysics Data System (ADS)

    Tauris, Thomas M.; Langer, Norbert; Podsiadlowski, Philipp

    2015-08-01

    The explosion of ultra-stripped stars in close binaries can lead to ejecta masses <0.1 M⊙ and may explain some of the recent discoveries of weak and fast optical transients. In Tauris et al., it was demonstrated that helium star companions to neutron stars (NSs) may experience mass transfer and evolve into naked ˜1.5 M⊙ metal cores, barely above the Chandrasekhar mass limit. Here, we elaborate on this work and present a systematic investigation of the progenitor evolution leading to ultra-stripped supernovae (SNe). In particular, we examine the binary parameter space leading to electron-capture (EC SNe) and iron core-collapse SNe (Fe CCSNe), respectively, and determine the amount of helium ejected with applications to their observational classification as Type Ib or Type Ic. We mainly evolve systems where the SN progenitors are helium star donors of initial mass MHe = 2.5-3.5 M⊙ in tight binaries with orbital periods of Porb = 0.06-2.0 d, and hosting an accreting NS, but we also discuss the evolution of wider systems and of both more massive and lighter - as well as single - helium stars. In some cases, we are able to follow the evolution until the onset of silicon burning, just a few days prior to the SN explosion. We find that ultra-stripped SNe are possible for both EC SNe and Fe CCSNe. EC SNe only occur for MHe = 2.60-2.95 M⊙ depending on Porb. The general outcome, however, is an Fe CCSN above this mass interval and an ONeMg or CO white dwarf for smaller masses. For the exploding stars, the amount of helium ejected is correlated with Porb - the tightest systems even having donors being stripped down to envelopes of less than 0.01 M⊙. We estimate the rise time of ultra-stripped SNe to be in the range 12 h-8 d, and light-curve decay times between 1 and 50 d. A number of fitting formulae for our models are provided with applications to population synthesis. Ultra-stripped SNe may produce NSs in the mass range 1.10-1.80 M⊙ and are highly relevant for

  19. Ultra-fast ipsilateral DPOAE adaptation not modulated by attention?

    NASA Astrophysics Data System (ADS)

    Dalhoff, Ernst; Zelle, Dennis; Gummer, Anthony W.

    2018-05-01

    Efferent stimulation of outer hair cells is supposed to attenuate cochlear amplification of sound waves and is accompanied by reduced DPOAE amplitudes. Recently, a method using two subsequent f2 pulses during presentation of a longer f1 pulse was introduced to measure fast ipsilateral adaptation effects on separated DPOAE components. Compensating primary-tone onsets for their latencies at the f2-tonotopic place, the average adaptation measured in four normal-hearing subjects was 5.0 dB with a time constant below 5 ms. In the present study, two experiments were performed to determine the origin of this ultra-fast ipsilateral adaptation effect. The first experiment measured ultra-fast ipsilateral adaptation using a two-pulse paradigm at three frequencies in the four subjects, while controlling for visual attention of the subjects. The other experiment also controlled for visual attention, but utilized a sequence of f2 short pulses in the presence of a continuous f1 tone to sample ipsilateral adaptation effects with longer time constants in eight subjects. In the first experiment, no significant change in the ultra-fast adaptation between non-directed attention and visual attention could be detected. In contrast, the second experiment revealed significant changes in the magnitude of the slower ipsilateral adaptation in the visual-attention condition. In conclusion, the lack of an attentional influence indicates that the ultra-fast ipsilateral DPOAE adaptation is not solely mediated by the medial olivocochlear reflex.

  20. The UltraLightweight Technology for Research in Astronomy (ULTRA) Project

    NASA Astrophysics Data System (ADS)

    Twarog, B. A.; Anthony-Twarog, B. J.; Shawl, S. J.; Hale, R.; Taghavi, R.; Fesen, R.; Etzel, P. B.; Martin, R.; Romeo, R.

    2004-12-01

    The collaborative focus of four academic departments (Univ. of Kansas Aerospace Engineering, Univ. of Kansas Physics & Astronomy, San Diego State University Astronomy and Dartmouth College Astronomy) and a private industry partner (Composite Mirror Applications, Inc.-CMA, Inc.) is a three-year plan to develop and test UltraLightweight Technology for Research in Astronomy (ULTRA). The ULTRA technology, using graphite fiber composites to fabricate mirrors and telescope structures, offers a versatile and cost-effective tool for optical astronomy, including the economical fabrication and operation of telescopes ranging from small (1m or smaller) aperture for education and research to extremely large (30m+) segmented telescopes (ELTs). The specific goal of this NSF-funded three-year Major Research Instrumentation project is to design, build, and test a 1m-class optical tube assembly (OTA) and mirrors constructed entirely from composites. In the first year of the project, the team has built and is field-testing two 0.4m prototypes to validate the optical surfaces and figures of the mirrors and to test and refine the structural dynamics of the OTA. Preparation for design and construction of the 1m telescope is underway. When completed in late 2005, the ULTRA telescope will be operated remotely from Mt. Laguna Observatory east of San Diego, where it will undergo a period of intensive optical and imaging tests. A 0.4m prototype OTA with mirrors (12 kg total weight) will be on display at the meeting. Support of this work by NSF through grants AST-0320784 and AST-0321247, NASA grant NCC5-600, the University of Kansas, and San Diego State University is gratefully acknowledged.

  1. Position-specific automated processing of V3 env ultra-deep pyrosequencing data for predicting HIV-1 tropism

    PubMed Central

    Jeanne, Nicolas; Saliou, Adrien; Carcenac, Romain; Lefebvre, Caroline; Dubois, Martine; Cazabat, Michelle; Nicot, Florence; Loiseau, Claire; Raymond, Stéphanie; Izopet, Jacques; Delobel, Pierre

    2015-01-01

    HIV-1 coreceptor usage must be accurately determined before starting CCR5 antagonist-based treatment as the presence of undetected minor CXCR4-using variants can cause subsequent virological failure. Ultra-deep pyrosequencing of HIV-1 V3 env allows to detect low levels of CXCR4-using variants that current genotypic approaches miss. However, the computation of the mass of sequence data and the need to identify true minor variants while excluding artifactual sequences generated during amplification and ultra-deep pyrosequencing is rate-limiting. Arbitrary fixed cut-offs below which minor variants are discarded are currently used but the errors generated during ultra-deep pyrosequencing are sequence-dependant rather than random. We have developed an automated processing of HIV-1 V3 env ultra-deep pyrosequencing data that uses biological filters to discard artifactual or non-functional V3 sequences followed by statistical filters to determine position-specific sensitivity thresholds, rather than arbitrary fixed cut-offs. It allows to retain authentic sequences with point mutations at V3 positions of interest and discard artifactual ones with accurate sensitivity thresholds. PMID:26585833

  2. Position-specific automated processing of V3 env ultra-deep pyrosequencing data for predicting HIV-1 tropism.

    PubMed

    Jeanne, Nicolas; Saliou, Adrien; Carcenac, Romain; Lefebvre, Caroline; Dubois, Martine; Cazabat, Michelle; Nicot, Florence; Loiseau, Claire; Raymond, Stéphanie; Izopet, Jacques; Delobel, Pierre

    2015-11-20

    HIV-1 coreceptor usage must be accurately determined before starting CCR5 antagonist-based treatment as the presence of undetected minor CXCR4-using variants can cause subsequent virological failure. Ultra-deep pyrosequencing of HIV-1 V3 env allows to detect low levels of CXCR4-using variants that current genotypic approaches miss. However, the computation of the mass of sequence data and the need to identify true minor variants while excluding artifactual sequences generated during amplification and ultra-deep pyrosequencing is rate-limiting. Arbitrary fixed cut-offs below which minor variants are discarded are currently used but the errors generated during ultra-deep pyrosequencing are sequence-dependant rather than random. We have developed an automated processing of HIV-1 V3 env ultra-deep pyrosequencing data that uses biological filters to discard artifactual or non-functional V3 sequences followed by statistical filters to determine position-specific sensitivity thresholds, rather than arbitrary fixed cut-offs. It allows to retain authentic sequences with point mutations at V3 positions of interest and discard artifactual ones with accurate sensitivity thresholds.

  3. Memory and consciousness: trace distinctiveness in memory retrievals.

    PubMed

    Brunel, Lionel; Oker, Ali; Riou, Benoit; Versace, Rémy

    2010-12-01

    The aim of this article was to provide experimental evidence that classical dissociation between levels of consciousness associated with memory retrieval (i.e., implicit or explicit) can be explained in terms of task dependency and distinctiveness of traces. In our study phase, we manipulated the level of isolation (partial vs. global) of the memory trace by means of an isolation paradigm (isolated words among non-isolated words). We then tested these two types of isolation in a series of tasks of increasing complexity: a lexical decision task, a recognition task, and a free recall task. The main result of this study was that distinctiveness effects were observed as a function of the type of isolation (level of isolation) and the nature of the task. We concluded that trace distinctiveness improves subsequent access to the trace, while the level of trace distinctiveness also appears to determine the possibility of conscious or explicit retrieval. Copyright © 2010 Elsevier Inc. All rights reserved.

  4. Trace fossils as environment indicators in the Rocky Mountains

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

    Shepard, B.

    Throughout time, organisms have left various types of traces while engaged in different activities. The two major types of lebensspuren were made by suspension feeders found in turbulent water where organic matter is held in suspension, and by deposit feeders whose habitat is found in quiet, deeper waters where large quantities of organic matter settle from suspension. The different activities which occur in these two environments are the cause of the traces found in sediments. These include escape structures resulting from degradation or aggradation of sediments, feeding structures, dwelling structures, grazing traces, crawling traces, and resting traces. The use ofmore » trace fossils in hydrocarbon exploration is especially helpful in the Cretaceous sandstones of the Rocky Mountains because of the relative abundance of outcrops and the scarcity of body fossils. By combining the interpretation of physical processes with the biological traces, one more tool is made available in the determination of rock environments as an aid in hydrocarbon exploration. Materials exhibited include 8 x 10 color prints of different Cretaceous lebensspuren, hand-drawn cartoons of the six different trace activities, and a regional cross section of the Eagle sandstone illustrated by photographs of different traces near each location, as well as a variety of rock samples.« less

  5. Determination of Trace Elements in Edible Nuts in the Beijing Market by ICP-M.

    PubMed

    Yin, Liang Liang; Tian, Qing; Shao, Xian Zhang; Kong, Xiang Yin; Ji, Yan Qin

    2015-06-01

    Nuts have received increased attention from the public in recent years as important sources of some essential elements, and information on the levels of elements in edible nuts is useful to consumers. Determination of the elemental distributions in nuts is not only necessary in evaluating the total dietary intake of the essential elements, but also useful in detecting heavy metal contamination in food. The aim of this study was to determine the mineral contents in edible nuts, and to assess the food safety of nuts in the Beijing market. Levels of Li, Cr, Mn, Co, Cu, Zn, As, Se, Rb, Sr, Mo, Cd, Cs, Ba, Pb, Th, and U in 11 types of edible nuts and seeds (macadamia nuts, lotus nuts, pistachios, sunflower seeds, pine nuts, almonds, walnuts, chestnuts, hazelnuts, cashews, and ginkgo nuts) as well as raisins were determined by inductively coupled plasma mass spectrometry (ICP-MS). The accuracy of the method was validated using standard reference materials GBW10014 (cabbage) and GBW10016 (tea). Our results provide useful information for evaluating the levels of trace elements in edible nuts in the Beijing market, will be helpful for improving food safety, and will aid in better protecting consumer interests. Copyright © 2015 The Editorial Board of Biomedical and Environmental Sciences. Published by China CDC. All rights reserved.

  6. Determination of trace endocrine active phenolic compounds by GC/MS

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

    Gang Sun; Geno, P.W.

    1997-12-31

    4-Nonylphenol ethoxylates (NPEOs) and 4-octylphenol ethoxylates (OPEOs) are widely used as nonionic surfactants, Due to the potential estrogenic properties of these compounds and their biodegradation products, there is increasing concern about their presence in ground and drinking water. To assess their prevalence in drinking and ground water, a simple, highly sensitive and accurate analytical method for determination of trace amounts of 4-nonylphenol, 4-nonylphenol monoethoxylate (NP1EO), 4-nonylphenol diethoxylate (NP2EO), 4-nonylphenol monoethoxycarboxylate (NP1EC), 4-octylphenol, 4-octylphenol monoethoxylate (OP1EO), 4-octylphenol diethoxylate (OP2EO), and other 15 phenolic compounds has been developed and validated. One liter of drinking water sample was extracted and concentrated into dichloromethane.more » The analytes in the extracts were converted to their trimethylsilyl derivatives by reacting with N,O-bis(trimethylsilyl) trifluoroacetamine (BSTFA) and 10 % trimethylchlorosilane (TMCS) at 90{degrees}C. The derivatized extracts were then directly analyzed by gas chromatography-mass spectrometry operating in a selected-ion monitoring mode (GUMS-SIM). Method detection limits (MDLs) were 0.01 to 0.02 {mu}g/L for 4-nonylphenol, NP1EO, 2PNEO; 0.064 {mu}g/L for NP1EC; 0.005 to 0.02 {mu}g/L for 4-octylphenol, OP1EO, OP2EO; and 0.001 to 0.003 {mu}g/L, for other 15 phenolic compounds.« less

  7. A high-throughput solid-phase extraction microchip combined with inductively coupled plasma-mass spectrometry for rapid determination of trace heavy metals in natural water.

    PubMed

    Shih, Tsung-Ting; Hsieh, Cheng-Chuan; Luo, Yu-Ting; Su, Yi-An; Chen, Ping-Hung; Chuang, Yu-Chen; Sun, Yuh-Chang

    2016-04-15

    Herein, a hyphenated system combining a high-throughput solid-phase extraction (htSPE) microchip with inductively coupled plasma-mass spectrometry (ICP-MS) for rapid determination of trace heavy metals was developed. Rather than performing multiple analyses in parallel for the enhancement of analytical throughput, we improved the processing speed for individual samples by increasing the operation flow rate during SPE procedures. To this end, an innovative device combining a micromixer and a multi-channeled extraction unit was designed. Furthermore, a programmable valve manifold was used to interface the developed microchip and ICP-MS instrumentation in order to fully automate the system, leading to a dramatic reduction in operation time and human error. Under the optimized operation conditions for the established system, detection limits of 1.64-42.54 ng L(-1) for the analyte ions were achieved. Validation procedures demonstrated that the developed method could be satisfactorily applied to the determination of trace heavy metals in natural water. Each analysis could be readily accomplished within just 186 s using the established system. This represents, to the best of our knowledge, an unprecedented speed for the analysis of trace heavy metal ions. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. [Simultaneous determination of delta-9-tetrahydrocannabinol cannabidiol and cannabinol in edible oil using ultra performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Zhang, Aizhi; Wang, Quanlin; Mo, Shijie

    2010-11-01

    A method for the simultaneous determination of delta-9-tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in edible oil was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted with methanol, purified by an LC-Alumina-N solid phase extraction cartridge, separated and detected by the UPLC-MS/MS. Quantitative analysis was corrected by an isotope internal standard method using delta-9-THC-D3 as internal standard. Average recoveries for the target compounds varied from 68.0% to 101.6% with the relative standard deviations ranging from 7.0% to 20.1% at three spiked levels. The limits of detection (LOD) of the method were from 0.06-0.17 microg/kg and the limits of quantification (LOQ) were in the range of 0.20-0.52 microg/kg. The results showed that the method is able to meet the requirements for the simultaneous determination of THC, CBD and CBN in edible oil.

  9. Ultra Reliability Workshop Introduction

    NASA Technical Reports Server (NTRS)

    Shapiro, Andrew A.

    2006-01-01

    This plan is the accumulation of substantial work by a large number of individuals. The Ultra-Reliability team consists of representatives from each center who have agreed to champion the program and be the focal point for their center. A number of individuals from NASA, government agencies (including the military), universities, industry and non-governmental organizations also contributed significantly to this effort. Most of their names may be found on the Ultra-Reliability PBMA website.

  10. Electroadsorption-assisted direct determination of trace arsenic without interference using transmission X-ray fluorescence spectroscopy.

    PubMed

    Jiang, Tian-Jia; Guo, Zheng; Liu, Jin-Huai; Huang, Xing-Jiu

    2015-08-18

    An analytical technique based on electroadsorption and transmission X-ray fluorescence (XRF) for the quantitative determination of arsenic in aqueous solution with ppb-level limits of detection (LOD) is proposed. The approach uses electroadsorption to enhance the sensitivity and LOD of the arsenic XRF response. Amine-functionalized carbonaceous microspheres (NH2-CMSs) are found to be the ideal materials for both the quantitative adsorption of arsenic and XRF analysis due to the basic amine sites on the surface and their noninterference in the XRF spectrum. In electroadsorptive X-ray fluorescence (EA-XRF), arsenic is preconcentrated by a conventional three-electrode system with a positive electricity field around the adsorbents. Then, the quantification of arsenic on the adsorbents is achieved using XRF. The electroadsorption preconcentration can realize the fast transfer of arsenic from the solution to the adsorbents and improve the LOD of conventional XRF compared with directly determining arsenic solution by XRF alone. The sensitivity of 0.09 cnt ppb(-1) is obtained without the interferences from coexisted metal ions in the determination of arsenic, and the LOD is found to be 7 ppb, which is lower than the arsenic guideline value of 10 ppb given by the World Health Organization (WHO). These results demonstrated that XRF coupled with electroadsorption was able to determine trace arsenic in real water sample.

  11. Ultra-high pressure LC for astaxanthin determination in shrimp by-products and active food packaging.

    PubMed

    Sanches-Silva, A; Ribeiro, T; Albuquerque, T G; Paseiro, P; Sendón, R; de Quirós, A Bernaldo; López-Cervantes, J; Sánchez-Machado, D I; Soto Valdez, H; Angulo, I; Aurrekoetxea, G P; Costa, H S

    2013-06-01

    Nowadays, there is increasing interest in natural antioxidants from food by-products. Astaxanthin is a potent antioxidant and one of the major carotenoids in crustaceans and salmonids. An ultra-high pressure liquid chromatographic method was developed and validated for the determination of astaxanthin in shrimp by-products, and its migration from new packaging materials to food simulants was also studied. The method uses an UPLC® BEH guard-column (2.1 × 5 mm, 1.7 µm particle size) and an UPLC® BEH analytical column (2.1 × 50 mm, 1.7 µm particle size). Chromatographic separation was achieved using a programmed gradient mobile phase consisting of (A) acetonitrile-methanol (containing 0.05 m ammonium acetate)-dichloromethane (75:20:5, v/v/v) and (B) ultrapure water. This method was evaluated with respect to validation parameters such as linearity, precision, limit of detection, limit of quantification and recovery. Low-density polyethylene films were prepared with different amounts of the lipid fraction of fermented shrimp waste by extrusion, and migration was evaluated into food simulants (isooctane and ethanol 95%, v/v). Migration was not detected under the tested conditions. Copyright © 2012 John Wiley & Sons, Ltd.

  12. Application of ultra-high performance supercritical fluid chromatography for the determination of carotenoids in dietary supplements.

    PubMed

    Li, Bing; Zhao, Haiyan; Liu, Jing; Liu, Wei; Fan, Sai; Wu, Guohua; Zhao, Rong

    2015-12-18

    A quick and simple ultra-high performance supercritical fluid chromatography-photodiode array detector method was developed and validated for the simultaneous determination of 9 carotenoids in dietary supplements. The influences of stationary phase, co-solvent, pressure, temperature and flow rate on the separation of carotenoids were evaluated. The separation of the carotenoids was carried out using an Acquity UPC(2) HSS C18 SB column (150mm×3.0mm, 1.8μm) by gradient elution with carbon dioxide and a 1:2 (v:v) methanol/ethanol mixture. The column temperature was set to 35°C and the backpressure was 15.2MPa. Under these conditions, 9 carotenoids and the internal standard, β-apo-8'-carotenal, were successfully separated within 10min. The correlation coefficients (R(2)) of the calibration curves were all above 0.997, the limits of detection for the 9 carotenoids were in the range of 0.33-1.08μg/mL, and the limits of quantification were in the range of 1.09-3.58μg/mL. The mean recoveries were from 93.4% to 109.5% at different spiking levels, and the relative standard deviations were between 0.8% and 6.0%. This method was successfully applied to the determination of 9 carotenoids in commercial dietary supplements. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Ultra-processed foods and added sugars in the Chilean diet (2010).

    PubMed

    Cediel, Gustavo; Reyes, Marcela; da Costa Louzada, Maria Laura; Martinez Steele, Euridice; Monteiro, Carlos A; Corvalán, Camila; Uauy, Ricardo

    2018-01-01

    To assess the consumption of ultra-processed foods and analyse its association with the content of added sugars in the Chilean diet. Cross-sectional study of national dietary data obtained through 24 h recalls and classified into food groups according to the extent and purpose of food processing (NOVA classification). Chile. A probabilistic sample of 4920 individuals (aged 2 years or above) studied in 2010 by a national dietary survey (Encuesta Nacional de Consumo Alimentario). Ultra-processed foods represented 28·6 (se 0·5) % of total energy intake and 58·6 (se 0·9) % of added sugars intake. The mean percentage of energy from added sugars increased from 7·7 (se 0·3) to 19·7 (se 0·5) % across quintiles of the dietary share of ultra-processed foods. After adjusting for several potential sociodemographic confounders, a 5 percentage point increase in the dietary share of ultra-processed foods determined a 1 percentage point increase in the dietary content of added sugars. Individuals in the highest quintile were three times more likely (OR=2·9; 95 % CI 2·4, 3·4) to exceed the 10 % upper limit for added sugars recommended by the WHO compared with those in the lowest quintile, after adjusting for sociodemographic variables. This association was strongest among individuals aged 2-19 years (OR=3·9; 95 % CI 2·7, 5·9). In Chile, ultra-processed foods are important contributors to total energy intake and to the consumption of added sugars. Actions aimed at limiting consumption of ultra-processed foods are being implemented as effective ways to achieve WHO dietary recommendations to limit added sugars and processed foods, especially for children and adolescents.

  14. Determination of ultra-short laser induced damage threshold of KH{sub 2}PO{sub 4} crystal: Numerical calculation and experimental verification

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

    Cheng, Jian; Department of Physics, The Ohio State University, 191 W. Woodruff Ave, Columbus, OH 43210; Chen, Mingjun, E-mail: chenmj@hit.edu.cn, E-mail: chowdhury.24@osu.edu

    Rapid growth and ultra-precision machining of large-size KDP (KH{sub 2}PO{sub 4}) crystals with high laser damage resistance are tough challenges in the development of large laser systems. It is of high interest and practical significance to have theoretical models for scientists and manufacturers to determine the laser-induced damage threshold (LIDT) of actually prepared KDP optics. Here, we numerically and experimentally investigate the laser-induced damage on KDP crystals in ultra-short pulse laser regime. On basis of the rate equation for free electron generation, a model dedicated to predicting the LIDT is developed by considering the synergistic effect of photoionization, impact ionizationmore » and decay of electrons. Laser damage tests are performed to measure the single-pulse LIDT with several testing protocols. The testing results combined with previously reported experimental data agree well with those calculated by the model. By taking the light intensification into consideration, the model is successfully applied to quantitatively evaluate the effect of surface flaws inevitably introduced in the preparation processes on the laser damage resistance of KDP crystals. This work can not only contribute to further understanding of the laser damage mechanisms of optical materials, but also provide available models for evaluating the laser damage resistance of exquisitely prepared optical components used in high power laser systems.« less

  15. Determination of trace tin by solid substrate-room temperature phosphorimetry using sodium dodecyl sulfate as sensitizer

    NASA Astrophysics Data System (ADS)

    Jiaming, Liu; Guohui, Zhu; Tianlong, Yang; Aihong, Wu; Yan, Fu; Longdi, Li

    2003-07-01

    The effects of different surfactants on solid substrate-room temperature phosphorescence (SS-RTP) properties of Sn4+-morin systems were investigated. It was found that the SS-RTP intensity of luminescence system was increased greatly in presence of sodium dodecyl sulfate (SDS). A new highly sensitive method for the determination of trace tin has been proposed based on sensitization of SDS on SS-RTP intensity of morin-tin system on the filter paper substrate. The linear dynamic range of this method is 8.0-112 ag per spot (with the volume of 0.4 μl per spot) with a detection limit of 4.0 ag per spot, and the regression equation is ΔIp=199.7+3.456mSn(IV) (ag per spot), with the correlation coefficient r=0.9998 (n=7). This simple, rapid and reproducible method has been applied to determine the amount of tin in real samples with satisfactory results.

  16. Back-extraction of trace elements from organometallic-halide extracts for determination by flameless atomic absorption spectrometry

    USGS Publications Warehouse

    Clark, J.R.; Viets, J.G.

    1981-01-01

    The Methyl isobutyl ketone-Amine synerGistic Iodkte Complex (MAGIC) extraction system offers the advantage that a large number of trace elements can be rapidly determined with a single sample preparation procedure. However, many of the elements extracted by the MAGIC system form volatile organometallic halide salts when the organic extract is heated in the graphite furnace. High concentrations of some elements such as Cu and Zn extracted by the system from anomalous geological samples produce serious interferences when certain other elements are determined by flameless atomic absorption. Stripping systems have been developed using solutions of HNO3, H2SO4, and CH3COOH individually or combined with H2O2 in order to circumvent these problems. With these systems most of the elements in the organic extract can be sequentially stripped into an aqueous phase. Organometallic volatilization and the most serious interelement interferences, therefore, can be eliminated by stripping with various combinations of reagents in a series of steps.

  17. Evaluation of trace element status of organic dairy cattle.

    PubMed

    Orjales, I; Herrero-Latorre, C; Miranda, M; Rey-Crespo, F; Rodríguez-Bermúdez, R; López-Alonso, M

    2018-06-01

    The present study aimed to evaluate trace mineral status of organic dairy herds in northern Spain and the sources of minerals in different types of feed. Blood samples from organic and conventional dairy cattle and feed samples from the respective farms were analysed by inductively coupled plasma mass spectrometry to determine the concentrations of the essential trace elements (cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), iodine (I), manganese (Mn), molybdenum (Mo), nickel (Ni), selenium (Se) and zinc (Zn)) and toxic trace elements (arsenic (As), cadmium (Cd), mercury (Hg) and lead (Pb)). Overall, no differences between organic and conventional farms were detected in serum concentrations of essential and toxic trace elements (except for higher concentrations of Cd on the organic farms), although a high level of inter-farm variation was detected in the organic systems, indicating that organic production greatly depends on the specific local conditions. The dietary concentrations of the essential trace elements I, Cu, Se and Zn were significantly higher in the conventional than in the organic systems, which can be attributed to the high concentration of these minerals in the concentrate feed. No differences in the concentrations of trace minerals were found in the other types of feed. Multivariate chemometric analysis was conducted to determine the contribution of different feed sources to the trace element status of the cattle. Concentrate samples were mainly associated with Co, Cu, I, Se and Zn (i.e. with the elements supplemented in this type of feed). However, pasture and grass silage were associated with soil-derived elements (As, Cr, Fe and Pb) which cattle may thus ingest during grazing.

  18. Determination of gallium at trace levels using a spectrofluorimetric method in synthetic U-Ga and Ga-As solutions.

    PubMed

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

    2010-01-01

    A simple, easy to use and selective spectrofluorimetric method for the determination of trace levels of gallium has been developed. A new Schiff base, N-o-vanillidine-2-amino-p-cresol (OVAC) was synthesized and its fluorescence activity with gallium investigated. Based on this chelation reaction, a spectrofluorimetric method has been developed for the determination of gallium in synthetically prepared Ga-U and Ga-As samples buffered at pH 4.0 using acetic acid-sodium acetate. The chelation reaction between Ga(III) and N-o-vanillidine-2-amino-p-cresol was very fast, requiring only 30min at room temperature to complex completely. The limit of detection (LOD) (3sigma) for Ga(III) was 7.17 nM (0.50 microgL(-1)), determined from the analysis of 11 different solutions of 20 microg L(-1) Ga(III). Copyright 2009 Elsevier B.V. All rights reserved.

  19. Structural performance of ultra-thin whitetopping on Illinois roadways and parking lots.

    DOT National Transportation Integrated Search

    2014-08-01

    A performance evaluation of ultra-thin whitetopping (UTW) pavements in Illinois was undertaken in 20122014 : to evaluate current design procedures and to determine design life criteria for future projects. The two main : components of this evaluat...

  20. Spacelab baseline ECS trace contaminant removal test program

    NASA Technical Reports Server (NTRS)

    Ray, C. D.; Stanley, J. B.

    1977-01-01

    An estimate of the Spacelab Baseline Environmental Control System's contaminated removal capability was required to allow determination of the need for a supplemental trace contaminant removal system. Results from a test program to determine this removal capability are presented.

  1. Characterisation of baroreflex sensitivity of recreational ultra-endurance athletes.

    PubMed

    Foulds, Heather J A; Cote, Anita T; Phillips, Aaron A; Charlesworth, Sarah A; Bredin, Shannon S D; Burr, Jamie F; Drury, Chipman Taylor; Ngai, Shirley; Fougere, Renee J; Ivey, Adam C; Warburton, Darren E R

    2014-01-01

    Altered autonomic function has been identified following ultra-endurance event participation among elite world-class athletes. Despite dramatic increases in recreational athlete participation in these ultra-endurance events, the physiological effects on these athletes are less known. This investigation sought to characterise changes in surrogate measures of autonomic function: heart rate variability (HRV), blood pressure variability (BPV) and baroreceptor sensitivity (BRS) following ultra-endurance race participation. Further, we sought to compare baseline measures among ultra-endurance athletes and recreationally active controls not participating in the ultra-endurance race. Recreational ultra-endurance athletes (n = 25, 44.6 ± 8.2 years, 8 females) and recreationally active age, sex and body mass index matched controls (n = 25) were evaluated. Measurements of HRV, BPV and BRS were collected pre- and post-race for recreational ultra-endurance athletes and at baseline, for recreationally active controls. Post-race, ultra-endurance athletes demonstrated significantly greater sympathetic modulation [low frequency (LF) power HRV: 50.3 ± 21.6 normalised units (n.u.) to 65.9 ± 20.4 n.u., p = 0.01] and significantly lower parasympathetic modulation [high frequency (HF) power HRV: 45.0 ± 22.4 n.u. to 23.9 ± 13.1 n.u., p < 0.001] and BRS. Baseline measurements BRS (spectral: 13.96 ± 10.82 ms·mmHg(-1) vs. 11.39 ± 5.33 ms·mmHg(-1)) were similar among recreational ultra-endurance athletes and recreationally active controls, though recreational ultra-endurance athletes demonstrated greater parasympathetic modulation of some HRV and BPV measures. Recreational ultra-endurance athletes experienced increased sympathetic tone and declines in BRS post-race, similar to previously reported elite world-class ultra-endurance athletes, though still within normal population ranges.

  2. Chemically individual armoured bioreporter bacteria used for the in vivo sensing of ultra-trace toxic metal ions.

    PubMed

    Zhang, Zhijun; Ju, Enguo; Bing, Wei; Wang, Zhenzhen; Ren, Jinsong; Qu, Xiaogang

    2017-07-25

    A chemically engineered armour is developed for simultaneously improving bioreporter bacterial vitality and shielding infectivity. The armour can help bacteria to resist various insults and even immune phagocytosis. Meanwhile, the bacterial infectivity has proven to be greatly shielded as well. Most importantly, the original bacterial biosensing activity is well preserved, which is competent for sensing trace arsenic in water, serum, and even in vivo.

  3. TraceContract

    NASA Technical Reports Server (NTRS)

    Kavelund, Klaus; Barringer, Howard

    2012-01-01

    TraceContract is an API (Application Programming Interface) for trace analysis. A trace is a sequence of events, and can, for example, be generated by a running program, instrumented appropriately to generate events. An event can be any data object. An example of a trace is a log file containing events that a programmer has found important to record during a program execution. Trace - Contract takes as input such a trace together with a specification formulated using the API and reports on any violations of the specification, potentially calling code (reactions) to be executed when violations are detected. The software is developed as an internal DSL (Domain Specific Language) in the Scala programming language. Scala is a relatively new programming language that is specifically convenient for defining such internal DSLs due to a number of language characteristics. This includes Scala s elegant combination of object-oriented and functional programming, a succinct notation, and an advanced type system. The DSL offers a combination of data-parameterized state machines and temporal logic, which is novel. As an extension of Scala, it is a very expressive and convenient log file analysis framework.

  4. Modeling Bloch oscillations in ultra-small Josephson junctions

    NASA Astrophysics Data System (ADS)

    Vora, Heli; Kautz, Richard; Nam, Sae Woo; Aumentado, Jose

    In a seminal paper, Likharev et al. developed a theory for ultra-small Josephson junctions with Josephson coupling energy (Ej) less than the charging energy (Ec) and showed that such junctions demonstrate Bloch oscillations which could be used to make a fundamental current standard that is a dual of the Josephson volt standard. Here, based on the model of Geigenmüller and Schön, we numerically calculate the current-voltage relationship of such an ultra-small junction which includes various error processes present in a nanoscale Josephson junction such as random quasiparticle tunneling events and Zener tunneling between bands. This model allows us to explore the parameter space to see the effect of each process on the width and height of the Bloch step and serves as a guide to determine whether it is possible to build a quantum current standard of a metrological precision using Bloch oscillations.

  5. Determination of trace quaternary ammonium surfactants in water by combining solid-phase extraction with surface-assisted laser desorption/ionization mass spectrometry.

    PubMed

    Chen, Y C; Sun, M C

    2001-01-01

    This study demonstrates the feasibility of combining solid-phase extraction (SPE) with surface-assisted laser desorption/ionization (SALDI) mass spectrometry to determine trace quaternary ammonium surfactants in water. The trace surfactants in water were directly concentrated on the surface of activated carbon sorbent in SPE. The activated carbon sorbent was then mixed with the SALDI liquid for SALDI analysis. No SPE elution procedure was necessary. Experimental results indicate that the surfactants with longer chain alkyl groups exhibit higher sensitivities than those with shorter chain alkyl groups in SPE-SALDI analysis. The detection limit for hexadecyltrimethylammonium bromide is around 10 ppt in SPE-SALDI analysis by sampling 100 mL of aqueous solution, while that of tetradecyltrimethylammonium bromide is about 100 ppt. The detection limit for decyltrimethylammonium bromide and dodecyltrimethylammonium bromide is in the low-ppb range. Copyright 2001 John Wiley & Sons, Ltd.

  6. Coexistence of colossal stress and texture gradients in sputter deposited nanocrystalline ultra-thin metal films

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

    Kuru, Yener; Welzel, Udo; Mittemeijer, Eric J.

    2014-12-01

    This paper demonstrates experimentally that ultra-thin, nanocrystalline films can exhibit coexisting colossal stress and texture depth gradients. Their quantitative determination is possible by X-ray diffraction experiments. Whereas a uniform texture by itself is known to generally cause curvature in so-called sin{sup 2}ψ plots, it is shown that the combined action of texture and stress gradients provides a separate source of curvature in sin{sup 2}ψ plots (i.e., even in cases where a uniform texture does not induce such curvature). On this basis, the texture and stress depth profiles of a nanocrystalline, ultra-thin (50 nm) tungsten film could be determined.

  7. Feasibility of UltraFast Doppler in Post-operative Evaluation of Hepatic Artery in Recipients following Liver Transplantation.

    PubMed

    Kim, Se-Young; Kim, Kyoung Won; Choi, Sang Hyun; Kwon, Jae Hyun; Song, Gi-Won; Kwon, Heon-Ju; Yun, Young Ju; Lee, Jeongjin; Lee, Sung-Gyu

    2017-11-01

    To determine the feasibility of using UltraFast Doppler in post-operative evaluation of the hepatic artery (HA) after liver transplantation (LT), we evaluated 283 simultaneous conventional and UltraFast Doppler sessions in 126 recipients over a 2-mo period after LT, using an Aixplorer scanner The Doppler indexes of the HA (peak systolic velocity [PSV], end-diastolic velocity [EDV], resistive index [RI] and systolic acceleration time [SAT]) by retrospective analysis of retrieved waves from UltraFast Doppler clips were compared with those obtained by conventional spectral Doppler. Correlation, performance in diagnosing the pathologic wave, examination time and reproducibility were evaluated. The PSV, EDV, RI and SAT of spectral and UltraFast Doppler measurements exhibited excellent correlation with favorable diagnostic performance. During the bedside examination, the mean time spent for UltraFast clip storing was significantly shorter than that for conventional Doppler US measurements. Both conventional and UltraFast Doppler exhibited good to excellent inter-analysis consistency. In conclusion, compared with conventional spectral Doppler, UltraFast Doppler values correlated excellently and yielded acceptable pathologic wave diagnostic performance with reduced examination time at the bedside and excellent reproducibility. Copyright © 2017 World Federation for Ultrasound in Medicine & Biology. Published by Elsevier Inc. All rights reserved.

  8. [Determination of arbutin in apple juice concentrate by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry].

    PubMed

    Kong, Xianghong; He, Qiang; Yue, Aishan; Wu, Shuangmin; Li, Jianhua

    2010-06-01

    An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) method was developed for the determination of arbutin in apple juice concentrate. Samples were diluted with water, then cleaned-up with a PS-DVB column. Quantitation was carried out using an external standard method. UPLC was performed on an Eclipse Plus C, column (100 mm x 2.1 mm, 1.8 microm) using a gradient solvent system (methanol-water). MS/MS was performed with multiple reaction monitoring (MRM) mode. The detection limit of arbutin was 0.02 mg/L. The method showed good linear relationship at the range of 0.04-2.0 mg/L. The recoveries ranged from 75.2% to 102.7% with relative standard deviations (RSDs) less than 8.9%. The method is simple, fast and sensitive. It's suitable for quantitative and qualitative analysis of arbutin in apple juice concentrate.

  9. Trace Elements in the Sea Surface Microlayer: Results from a Two Year Study in the Florida Keys

    NASA Astrophysics Data System (ADS)

    Ebling, A. M.; Westrich, J. R.; Lipp, E. K.; Mellett, T.; Buck, K. N.; Landing, W. M.

    2016-02-01

    Natural and anthropogenic aerosols are a significant source of trace elements to oligotrophic ocean surface waters, where they provide episodic pulses of limiting micronutrients for the microbial community. Opportunistic bacteria have been shown to experience rapid growth during deposition events. However, little is known about the fate of trace elements at the air-sea interface, i.e. the sea surface microlayer. It has been hypothesized that dust particles would be retained in the sea surface microlayer long enough to undergo chemical and physical changes that would affect the bioavailability of trace elements. In this study, aerosols, sea surface microlayer, and underlying water column samples were collected in the Florida Keys in July 2014 and May 2015 at various locations and analyzed for a suite of dissolved and particulate trace elements. Sea surface microlayer samples ( 50 μm) were collected using a cylinder of ultra-pure quartz glass; a novel adaptation of the glass plate technique. Sampling sites ranged from a more pristine environment approximately ten kilometers offshore to a more anthropogenic environment within a shallow bay a few hundred meters offshore. While it was clear from the results that dust deposition events played a large role in the chemical composition of the sea surface microlayer (elevated concentrations in dissolved and particulate trace elements associated with dust deposition), the location where the samples were collected also had a large impact on the sea surface microlayer as well as the underlying water column. The results were compared with other parameters analyzed such as Vibrio cultures as well as iron speciation, providing an important step towards our goal of understanding of the fate of trace elements in the sea surface microlayer as well as the specific effects of aeolian dust deposition on heterotrophic microbes in the upper ocean.

  10. Ray-trace analysis of glancing-incidence X-ray optical systems

    NASA Technical Reports Server (NTRS)

    Foreman, J. W., Jr.; Cardone, J. M.

    1976-01-01

    The results of a ray-trace analysis of several glancing-incidence X-ray optical systems are presented. The object of the study was threefold. First, the vignetting characteristics of the S-056 X-ray telescope were calculated using experimental data to determine mirror reflectivities. Second, a small Wolter Type I X-ray telescope intended for possible use in the Geostationary Operational Environmental Satellite program was designed and ray traced. Finally, a ray-trace program was developed for a Wolter-Schwarzschild X-ray telescope.

  11. The MESSIER surveyor: unveiling the ultra-low surface brightness universe

    NASA Astrophysics Data System (ADS)

    Valls-Gabaud, David; MESSIER Collaboration

    2017-03-01

    The MESSIER surveyor is a small mission designed at exploring the very low surface brightness universe. The satellite will drift-scan the entire sky in 6 filters covering the 200-1000 nm range, reaching unprecedented surface brightness levels of 34 and 37 mag arcsec-2 in the optical and UV, respectively. These levels are required to achieve the two main science goals of the mission: to critically test the ΛCDM paradigm of structure formation through (1) the detection and characterisation of ultra-faint dwarf galaxies, which are predicted to be extremely abundant around normal galaxies, but which remain elusive; and (2) tracing the cosmic web, which feeds dark matter and baryons into galactic haloes, and which may contain the reservoir of missing baryons at low redshifts. A large number of science cases, ranging from stellar mass loss episodes to intracluster light through fluctuations in the cosmological UV-optical background radiation are free by-products of the full-sky maps produced.

  12. 7 CFR 58.144 - Pasteurization or ultra-pasteurization.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Pasteurization or ultra-pasteurization. 58.144 Section... Service 1 Operations and Operating Procedures § 58.144 Pasteurization or ultra-pasteurization. When pasteurization or ultra-pasteurization is intended or required, or when a product is designated “pasteurized” or...

  13. Simultaneous determination and qualitative analysis of six types of components in Naoxintong capsule by miniaturized matrix solid-phase dispersion extraction coupled with ultra high-performance liquid chromatography with photodiode array detection and quadrupole time-of-flight mass spectrometry.

    PubMed

    Wang, Huilin; Jiang, Yan; Ding, Mingya; Li, Jin; Hao, Jia; He, Jun; Wang, Hui; Gao, Xiu-Mei; Chang, Yan-Xu

    2018-02-03

    A simple and effective sample preparation process based on miniaturized matrix solid-phase dispersion was developed for simultaneous determination of phenolic acids (gallic acid, chlorogenic acid, ferulic acid, 3,5-dicaffeoylqunic acid, 1,5-dicaffeoylqunic acid, rosmarinic acid, lithospermic acid, and salvianolic acid B), flavonoids (kaempferol-3-O-rutinoside, calycosin, and formononetin), lactones (ligustilide and butyllidephthalide), monoterpenoids (paeoniflorin), phenanthraquinones (cryptotanshinone), and furans (5-hydroxymethylfurfural) in Naoxintong capsule by ultra high-performance liquid chromatography. The optimized condition was that 25 mg Naoxintong powder was blended homogeneously with 100 mg Florisil PR for 4 min. One milliliter of methanol/water (75:25, v/v) acidified by 0.05% formic acid was selected to elute all components. It was found that the recoveries of the six types of components ranged from 61.36 to 96.94%. The proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography was successfully applied to simultaneous determination of the six types of components in Naoxintong capsules. The results demonstrated that the proposed miniaturized matrix solid-phase dispersion coupled with ultra high-performance liquid chromatography could be used as an environmentally friendly tool for the extraction and determination of multiple bioactive components in natural products. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Determination of minor and trace elements in kidney stones by x-ray fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Srivastava, Anjali; Heisinger, Brianne J.; Sinha, Vaibhav; Lee, Hyong-Koo; Liu, Xin; Qu, Mingliang; Duan, Xinhui; Leng, Shuai; McCollough, Cynthia H.

    2014-03-01

    The determination of accurate material composition of a kidney stone is crucial for understanding the formation of the kidney stone as well as for preventive therapeutic strategies. Radiations probing instrumental activation analysis techniques are excellent tools for identification of involved materials present in the kidney stone. In particular, x-ray fluorescence (XRF) can be very useful for the determination of minor and trace materials in the kidney stone. The X-ray fluorescence measurements were performed at the Radiation Measurements and Spectroscopy Laboratory (RMSL) of department of nuclear engineering of Missouri University of Science and Technology and different kidney stones were acquired from the Mayo Clinic, Rochester, Minnesota. Presently, experimental studies in conjunction with analytical techniques were used to determine the exact composition of the kidney stone. A new type of experimental set-up was developed and utilized for XRF analysis of the kidney stone. The correlation of applied radiation source intensity, emission of X-ray spectrum from involving elements and absorption coefficient characteristics were analyzed. To verify the experimental results with analytical calculation, several sets of kidney stones were analyzed using XRF technique. The elements which were identified from this techniques are Silver (Ag), Arsenic (As), Bromine (Br), Chromium (Cr), Copper (Cu), Gallium (Ga), Germanium (Ge), Molybdenum (Mo), Niobium (Nb), Rubidium (Rb), Selenium (Se), Strontium (Sr), Yttrium (Y), Zirconium (Zr). This paper presents a new approach for exact detection of accurate material composition of kidney stone materials using XRF instrumental activation analysis technique.

  15. Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches

    NASA Astrophysics Data System (ADS)

    Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

    2017-02-01

    A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu2 +), cobalt ions (Co2 +) and nickel ions (Ni2 +) mixture was 0.10 μg L- 1, 0.15 μg L- 1 and 0.13 μg L- 1, respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field.

  16. Laser-Induced Breakdown Spectroscopy of Trace Metals

    NASA Technical Reports Server (NTRS)

    Simons, Stephen (Technical Monitor); VanderWal, Randall L.; Ticich, Thomas M.; West, Joseph R., Jr.

    2004-01-01

    An alternative approach for laser-induced breakdown spectroscopy (LIBS) determination of trace metal determination in liquids is demonstrated. The limits of detection (LOD) for the technique ranged from 10 ppb to 10 ppm for 15 metals metals (Mg, Al, Si, Ca, Ti, Cr, Fe, Co, Ni, Cu, Zn, As, Cd, Hg, Pb) tested.

  17. Metabolic characteristics of keto-adapted ultra-endurance runners.

    PubMed

    Volek, Jeff S; Freidenreich, Daniel J; Saenz, Catherine; Kunces, Laura J; Creighton, Brent C; Bartley, Jenna M; Davitt, Patrick M; Munoz, Colleen X; Anderson, Jeffrey M; Maresh, Carl M; Lee, Elaine C; Schuenke, Mark D; Aerni, Giselle; Kraemer, William J; Phinney, Stephen D

    2016-03-01

    Many successful ultra-endurance athletes have switched from a high-carbohydrate to a low-carbohydrate diet, but they have not previously been studied to determine the extent of metabolic adaptations. Twenty elite ultra-marathoners and ironman distance triathletes performed a maximal graded exercise test and a 180 min submaximal run at 64% VO2max on a treadmill to determine metabolic responses. One group habitually consumed a traditional high-carbohydrate (HC: n=10, %carbohydrate:protein:fat=59:14:25) diet, and the other a low-carbohydrate (LC; n=10, 10:19:70) diet for an average of 20 months (range 9 to 36 months). Peak fat oxidation was 2.3-fold higher in the LC group (1.54±0.18 vs 0.67±0.14 g/min; P=0.000) and it occurred at a higher percentage of VO2max (70.3±6.3 vs 54.9±7.8%; P=0.000). Mean fat oxidation during submaximal exercise was 59% higher in the LC group (1.21±0.02 vs 0.76±0.11 g/min; P=0.000) corresponding to a greater relative contribution of fat (88±2 vs 56±8%; P=0.000). Despite these marked differences in fuel use between LC and HC athletes, there were no significant differences in resting muscle glycogen and the level of depletion after 180 min of running (-64% from pre-exercise) and 120 min of recovery (-36% from pre-exercise). Compared to highly trained ultra-endurance athletes consuming an HC diet, long-term keto-adaptation results in extraordinarily high rates of fat oxidation, whereas muscle glycogen utilization and repletion patterns during and after a 3 hour run are similar. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

  18. Trace Element Determination from the Guliya Ice Core to Characterize Aerosol Deposition over the Western Tibetan Plateau during the Last 500 Years

    NASA Astrophysics Data System (ADS)

    Sierra Hernandez, R.; Gabrielli, P.; Beaudon, E.; Wegner, A.; Thompson, L. G.

    2014-12-01

    The Tibetan Plateau or Third Pole covers over 5 million km2, and has ~46,000 glaciers that collectively contain one of the Earth's largest stores of fresh water. The Guliya ice cap located in the western Kunlun Shan on the Qinghai-Tibetan Plateau, China, is the largest (> 200 km2) ice cap in the subtropical zone. In 1992, a 308.6 m ice core to bedrock was recovered from the Guliya ice cap. The deepest 20 meters yielded the first record extending back through the last glacial cycle found outside of the Polar Regions. Because of its continental location on the northwestern side of the Tibetan Plateau, the atmospheric circulation over the Guliya ice cap is dominated by westerly air flow from the Eurasian region. Therefore the site is expected to be unaffected by the fallout of anthropogenic trace metals originating from the inner Asian continent and rather may serve to characterize trace metal emissions from the western countries. Here we present preliminary results of the determination of 29 trace elements, Rb, Sr, Nb, Mo, Ag, Cd, Sn, Sb, Cs, Ba, Ta, Tl, Pb, Bi, U, Li, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, and As, from Guliya ice core samples spanning the period 1500 - 1992 AD at seasonal (1750-1992 AD) and annual (1500-1750 AD) resolution. This Guliya trace element record will complement the developing records from the Dasuopu glacier, central Himalaya, and from the Puruogangri ice cap in the western Tanggula Shan in central Tibetan Plateau, which in contrast to Guliya are influenced by the monsoon. We investigate the possible sources both natural and anthropogenic of atmospheric trace elements and their fluxes over the Tibetan Plateau during the last 500 years.

  19. Application of polymer-coated glassy carbon electrodes to the direct determination of trace metals in body fluids by anodic tripping voltametry

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

    Hoyer, B.; Florence, T.M.

    This paper describes the use of a polymer-coated thin mercury film electrode for the direct determination of trace metals in body fluids by anodic stripping voltametry. The antifouling properties of the membrane coating greatly improve the analytical signal in comparison with the conventional thin mercury film electrode. Lead in whole blood, urine, and sweat and copper in sweat can be determined accurately with sample acidification as the only pretreatment step, while the determination of copper in serum requires sample deproteination prior to analysis. Owing to an improved procedure for the preparation of the perfluorosulfonated membrane, the lifetime of the electrodemore » is at least one working day when used continuously in acidified body fluids.« less

  20. Development of Hplc Techniques for the Analysis of Trace Metal Species in the Primary Coolant of a Pressurised Water Reactor.

    NASA Astrophysics Data System (ADS)

    Barron, Keiron Robert Philip

    Available from UMI in association with The British Library. The need to monitor corrosion products in the primary circuit of a pressurised water reactor (PWR), at a concentration of 10pg ml^{-1} is discussed. A review of trace and ultra-trace metal analysis, relevant to the specific requirements imposed by primary coolant chemistry, indicated that high performance liquid chromatography (HPLC), coupled with preconcentration of sample was an ideal technique. A HPLC system was developed to determine trace metal species in simulated PWR primary coolant. In order to achieve the desired detection limit an on-line preconcentration system had to be developed. Separations were performed on Aminex A9 and Benson BC-X10 analytical columns. Detection was by post column reaction with Eriochrome Black T and Calmagite Linear calibrations of 2.5-100ng of cobalt (the main species of interest), were achieved using up to 200ml samples. The detection limit for a 200ml sample was 10pg ml^{-1}. In order to achieve the desired aim of on-line collection of species at 300^circ C, the use of inorganic ion-exchangers is essential. A novel application, utilising the attractive features of the inorganic ion-exchangers titanium dioxide, zirconium dioxide, zirconium arsenophosphate and pore controlled glass beads, was developed for the preconcentration of trace metal species at temperature and pressure. The performance of these exchangers, at ambient and 300^ circC was assessed by their inclusion in the developed analytical system and by the use of radioisotopes. The particular emphasis during the development has been upon accuracy, reproducibility of recovery, stability of reagents and system contamination, studied by the use of radioisotopes and response to post column reagents. This study in conjunction with work carried out at Winfrith, resulted in a monitoring system that could follow changes in coolant chemistry, on deposition and release of metal species in simulated PWR water loops. On

  1. Ordering Traces Logically to Identify Lateness in Message Passing Programs

    DOE PAGES

    Isaacs, Katherine E.; Gamblin, Todd; Bhatele, Abhinav; ...

    2015-03-30

    Event traces are valuable for understanding the behavior of parallel programs. However, automatically analyzing a large parallel trace is difficult, especially without a specific objective. We aid this endeavor by extracting a trace's logical structure, an ordering of trace events derived from happened-before relationships, while taking into account developer intent. Using this structure, we can calculate an operation's delay relative to its peers on other processes. The logical structure also serves as a platform for comparing and clustering processes as well as highlighting communication patterns in a trace visualization. We present an algorithm for determining this idealized logical structure frommore » traces of message passing programs, and we develop metrics to quantify delays and differences among processes. We implement our techniques in Ravel, a parallel trace visualization tool that displays both logical and physical timelines. Rather than showing the duration of each operation, we display where delays begin and end, and how they propagate. As a result, we apply our approach to the traces of several message passing applications, demonstrating the accuracy of our extracted structure and its utility in analyzing these codes.« less

  2. Recoil-Implantation Of Multiple Radioisotopes Towards Wear Rate Measurements And Particle Tracing In Prosthetic Joints

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

    Warner, Jacob A.; Timmers, Heiko; Smith, Paul N.

    2011-06-01

    This study demonstrates a new method of radioisotope labeling of ultra-high molecular weight polyethylene inserts in prosthetic joints for wear studies. The radioisotopes {sup 97}Ru, {sup 100}Pd, {sup 100}Rh, and {sup 101m}Rh are produced in fusion evaporation reactions induced by {sup 12}C ions in a {sup 92}Zr target foil. The fusion products recoil-implant into ultra-high molecular weight polyethylene plugs, machined to fit into the surface of the inserts. During laboratory simulations of the joint motion, a wear rate of the labeled polyethylene may be measured and the pathways of wear debris particles can be traced by detecting characteristic gamma-rays. Themore » concentration profiles of the radioisotopes extend effectively uniformly from the polyethylene surface to a depth of about 4 {mu}m. The multiplicity of labeling and the use of several gamma-ray lines aids with avoiding systematic measurement uncertainties. Two polyethylene plugs were labeled and one was fitted into the surface of the tibial insert of a knee prosthesis, which had been worn in. Actuation over close to 100,000 cycles with a 900 N axial load and a 24 deg. flexion angle removed (14{+-}1)% of the gamma-ray activity from the plug. Most of this activity dispersed into the serum lubricant identifying this as the important debris pathway. Less than 1% activity was transferred to the femoral component of the prosthesis and the measured activity on the tibial tray was insignificant. Assuming uniform wear across the superior surface of the insert, a wear rate of (12{+-}3) mm{sup 3}/Megacycle was determined. This is consistent with wear rate measurements under similar conditions using other techniques.« less

  3. Ultra-wide-field imaging in diabetic retinopathy; an overview.

    PubMed

    Ghasemi Falavarjani, Khalil; Wang, Kang; Khadamy, Joobin; Sadda, Srinivas R

    2016-06-01

    To present an overview on ultra-wide-field imaging in diabetic retinopathy. A comprehensive search of the pubmed database was performed using the search terms of "ultra-wide-field imaging", "ultra-wide-field fluorescein angiography" and "diabetic retinopathy". The relevant original articles were reviewed. New advances in ultra-wide-field imaging allow for precise measurements of the peripheral retinal lesions. A consistent finding amongst these articles was that ultra-wide-field imaging improved detection of peripheral lesion. There was discordance among the studies, however, on the correlation between peripheral diabetic lesions and diabetic macular edema. Visualization of the peripheral retina using ultra-wide-field imaging improves diagnosis and classification of diabetic retinopathy. Additional studies are needed to better define the association of peripheral diabetic lesions with diabetic macular edema.

  4. [Measurement of the status of trace elements in cattle using liver biopsy samples].

    PubMed

    Ouweltjes, W; de Zeeuw, A C; Moen, A; Counotte, G H M

    2007-02-01

    Serum, plasma, or urine samples are usually used for the measurement of the trace elements copper; zinc, iron, selenium, because these samples are easy to obtain; however; these samples are not always appropriate. For example, it is not possible to measure molybdenum, the major antagonist of copper; in blood or urine. Therefore measurement of trace elements in liver tissue is considered the gold standard. For the assessment of selenium the method of choice remains determination of glutathion peroxidase in erythrocytes and for the assessment of magnesium determination of magnesium in urine. We determined the accuracy and repeatability of measuring trace elements in liver biopsies and whole liver homogenates. The levels of trace elements measured were similar in both preparations (92% agreement). Liver biopsy in live animals is a relatively simple procedure but not common in The Netherlands. Reference levels of trace elements, classified as too low, low, adequate, high, and too high, were established on the basis of our research and information in the literature. In a second study we investigated the practical aspects of obtaining liver tissue samples and their use. Samples were collected from cattle on a commercial dairy farm. Liver biopsy provided additional information to that obtained from serum and urine samples. We prepared a biopsy protocol and a test package, which we tested on 14 farms where an imbalance of trace minerals was suspected. Biopsy samples taken from 4 to 6 animals revealed extreme levels of trace elements.

  5. Determination of zircon/melt trace element partition coefficients from SIMS analysis of melt inclusions in zircon

    NASA Astrophysics Data System (ADS)

    Thomas, J. B.; Bodnar, R. J.; Shimizu, N.; Sinha, A. K.

    2002-09-01

    Partition coefficients ( zircon/meltD M) for rare earth elements (REE) (La, Ce, Nd, Sm, Dy, Er and Yb) and other trace elements (Ba, Rb, B, Sr, Ti, Y and Nb) between zircon and melt have been calculated from secondary ion mass spectrometric (SIMS) analyses of zircon/melt inclusion pairs. The melt inclusion-mineral (MIM) technique shows that D REE increase in compatibility with increasing atomic number, similar to results of previous studies. However, D REE determined using the MIM technique are, in general, lower than previously reported values. Calculated D REE indicate that light REE with atomic numbers less than Sm are incompatible in zircon and become more incompatible with decreasing atomic number. This behavior is in contrast to most previously published results which indicate D > 1 and define a flat partitioning pattern for elements from La through Sm. The partition coefficients for the heavy REE determined using the MIM technique are lower than previously published results by factors of ≈15 to 20 but follow a similar trend. These differences are thought to reflect the effects of mineral and/or glass contaminants in samples from earlier studies which employed bulk analysis techniques. D REE determined using the MIM technique agree well with values predicted using the equations of Brice (1975), which are based on the size and elasticity of crystallographic sites. The presence of Ce 4+ in the melt results in elevated D Ce compared to neighboring REE due to the similar valence and size of Ce 4+ and Zr 4+. Predicted zircon/meltD values for Ce 4+ and Ce 3+ indicate that the Ce 4+/Ce 3+ ratios of the melt ranged from about 10 -3 to 10 -2. Partition coefficients for other trace elements determined in this study increase in compatibility in the order Ba < Rb < B < Sr < Ti < Y < Nb, with Ba, Rb, B and Sr showing incompatible behavior (D M < 1.0), and Ti, Y and Nb showing compatible behavior (D M > 1.0). The effect of partition coefficients on melt evolution during

  6. Application of ray-traced tropospheric slant delays to geodetic VLBI analysis

    NASA Astrophysics Data System (ADS)

    Hofmeister, Armin; Böhm, Johannes

    2017-08-01

    The correction of tropospheric influences via so-called path delays is critical for the analysis of observations from space geodetic techniques like the very long baseline interferometry (VLBI). In standard VLBI analysis, the a priori slant path delays are determined using the concept of zenith delays, mapping functions and gradients. The a priori use of ray-traced delays, i.e., tropospheric slant path delays determined with the technique of ray-tracing through the meteorological data of numerical weather models (NWM), serves as an alternative way of correcting the influences of the troposphere on the VLBI observations within the analysis. In the presented research, the application of ray-traced delays to the VLBI analysis of sessions in a time span of 16.5 years is investigated. Ray-traced delays have been determined with program RADIATE (see Hofmeister in Ph.D. thesis, Department of Geodesy and Geophysics, Faculty of Mathematics and Geoinformation, Technische Universität Wien. http://resolver.obvsg.at/urn:nbn:at:at-ubtuw:1-3444, 2016) utilizing meteorological data provided by NWM of the European Centre for Medium-Range Weather Forecasts (ECMWF). In comparison with a standard VLBI analysis, which includes the tropospheric gradient estimation, the application of the ray-traced delays to an analysis, which uses the same parameterization except for the a priori slant path delay handling and the used wet mapping factors for the zenith wet delay (ZWD) estimation, improves the baseline length repeatability (BLR) at 55.9% of the baselines at sub-mm level. If no tropospheric gradients are estimated within the compared analyses, 90.6% of all baselines benefit from the application of the ray-traced delays, which leads to an average improvement of the BLR of 1 mm. The effects of the ray-traced delays on the terrestrial reference frame are also investigated. A separate assessment of the RADIATE ray-traced delays is carried out by comparison to the ray-traced delays from the

  7. On-site Determination of Trace Arsenic by Reflection-Absorption Colorimetry of Molybdenum Blue Collected on a Membrane Filter.

    PubMed

    Hasegawa, Yuya; Suzuki, Yasutada; Kawakubo, Susumu

    2017-01-01

    An on-site determination method for trace arsenic has been developed by collecting it as molybdenum blue (MB) in the presence of tetradecyldimethylbenzylammonium chloride on a mixed cellulose ester membrane filter and by measuring reflection absorbance (RA) of MB on the filter using a laboratory-made palm-top size reflection-absorbance colorimeter with a red light-emitting diode. The value of RA was proportional to the amount of arsenic up to 0.5 μg with a detection limit of 0.01 μg. The proposed method was successfully applied to soil extract and hot-spring water samples.

  8. Determination of permeability of ultra-fine cupric oxide aerosol through military filters and protective filters

    NASA Astrophysics Data System (ADS)

    Kellnerová, E.; Večeřa, Z.; Kellner, J.; Zeman, T.; Navrátil, J.

    2018-03-01

    The paper evaluates the filtration and sorption efficiency of selected types of military combined filters and protective filters. The testing was carried out with the use of ultra-fine aerosol containing cupric oxide nanoparticles ranging in size from 7.6 nm to 299.6 nm. The measurements of nanoparticles were carried out using a scanning mobility particle sizer before and after the passage through the filter and a developed sampling device at the level of particle number concentration approximately 750000 particles·cm-3. The basic parameters of permeability of ultra-fine aerosol passing through the tested material were evaluated, in particular particle size, efficiency of nanoparticle capture by filter, permeability coefficient and overall filtration efficiency. Results indicate that the military filter and particle filters exhibited the highest aerosol permeability especially in the nanoparticle size range between 100–200 nm, while the MOF filters had the highest permeability in the range of 200 to 300 nm. The Filter Nuclear and the Health and Safety filter had 100% nanoparticle capture efficiency and were therefore the most effective. The obtained measurement results have shown that the filtration efficiency over the entire measured range of nanoparticles was sufficient; however, it was different for particular particle sizes.

  9. Ultra-short ion and neutron pulse production

    DOEpatents

    Leung, Ka-Ngo; Barletta, William A.; Kwan, Joe W.

    2006-01-10

    An ion source has an extraction system configured to produce ultra-short ion pulses, i.e. pulses with pulse width of about 1 .mu.s or less, and a neutron source based on the ion source produces correspondingly ultra-short neutron pulses. To form a neutron source, a neutron generating target is positioned to receive an accelerated extracted ion beam from the ion source. To produce the ultra-short ion or neutron pulses, the apertures in the extraction system of the ion source are suitably sized to prevent ion leakage, the electrodes are suitably spaced, and the extraction voltage is controlled. The ion beam current leaving the source is regulated by applying ultra-short voltage pulses of a suitable voltage on the extraction electrode.

  10. Emission spectrographic determination of volatile trace elements in geologic materials by a carrier distillation technique

    USGS Publications Warehouse

    Barton, H.N.

    1986-01-01

    Trace levels of chalcophile elements that form volatile sulfide minerals are determined in stream sediments and in the nonmagnetic fraction of a heavy-mineral concentrate of stream sediments by a carrier distillation emission spectrographic method. Photographically recorded spectra of samples are visually compared with those of synthetic standards for the two sample types. Rock and soil samples may also be analyzed by comparison with the stream-sediment standards. A gallium oxide spectrochemical carrier/buffer enhances the early emission of the volatile elements. Detection limits in parts per million attained are: Sb 5, As 20, Bi 0.1, Cd 1, Cu 1, Pb 2, Ag 0.1, Zn 2, and Sn 0.1. A comparison with other methods of analysis, total-burn emission and atomic absorption spectroscopy, shows good correlation for standard reference for materials and samples from a variety of geologic terranes. ?? 1986.

  11. Trace elements in hazardous mineral fibres.

    PubMed

    Bloise, Andrea; Barca, Donatella; Gualtieri, Alessandro Francesco; Pollastri, Simone; Belluso, Elena

    2016-09-01

    Both occupational and environmental exposure to asbestos-mineral fibres can be associated with lung diseases. The pathogenic effects are related to the dimension, biopersistence and chemical composition of the fibres. In addition to the major mineral elements, mineral fibres contain trace elements and their content may play a role in fibre toxicity. To shed light on the role of trace elements in asbestos carcinogenesis, knowledge on their concentration in asbestos-mineral fibres is mandatory. It is possible that trace elements play a synergetic factor in the pathogenesis of diseases caused by the inhalation of mineral fibres. In this paper, the concentration levels of trace elements from three chrysotile samples, four amphibole asbestos samples (UICC amosite, UICC anthophyllite, UICC crocidolite and tremolite) and fibrous erionite from Jersey, Nevada (USA) were determined using inductively coupled plasma mass spectrometry (ICP-MS). For all samples, the following trace elements were measured: Li, Be, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, As, Rb, Sr, Y, Sb, Cs, Ba, La, Pb, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Th, U. Their distribution in the various mineral species is thoroughly discussed. The obtained results indicate that the amount of trace metals such as Mn, Cr, Co, Ni, Cu and Zn is higher in anthophyllite and chrysotile samples, whereas the amount of rare earth elements (REE) is higher in erionite and tremolite samples. The results of this work can be useful to the pathologists and biochemists who use asbestos minerals and fibrous erionite in-vitro studies as positive cyto- and geno-toxic standard references. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. Determination of naphthalene-derived compounds in apples by ultra-high performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Esparza, X; Moyano, E; Cosialls, J R; Galceran, M T

    2013-06-11

    Naphthylacetic acid, naphthyloxy acetic acid and naphthylacetamide belong to a group of synthetic substances known as "auxin-like" compounds which are used as growth regulators in vegetables and fruits due to their structure similarities with the indoleacetic acid, the most important plant auxin. This paper reports a selective, sensitive and fast ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the determination of naphthylacetamide (NAD) and the isomers (α and β) of naphthylacetic acid (NAA) and naphthyloxy acetic (NOA) acid in apple samples. A baseline separation between the respective isomers was achieved using an RP-Amide column with gradient elution. The UHPLC-MS/MS method developed, using electrospray and selected reaction monitoring (SRM) acquisition mode led to a reliable determination of these family of compounds in apple samples at low quantitation levels, down to 1.0 μg kg(-1) and 0.25 μg kg(-1) respectively. For confirmation of NAA accurate mass measurement is proposed giving at these conditions quantitation limits of 10 μg kg(-1) for this compound. The UHPLC-MS/MS method developed was used for the analysis of apple samples harvested in three different apple fields from Lleida (Spain) during the blooming period. NAD and NAA were found in samples collected during 4-5 weeks after application at concentrations between the quantification limits and 43 μg kg(-1) and 24 μg kg(-1), respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Massively parallel sensing of trace molecules and their isotopologues with broadband subharmonic mid-infrared frequency combs

    NASA Astrophysics Data System (ADS)

    Muraviev, A. V.; Smolski, V. O.; Loparo, Z. E.; Vodopyanov, K. L.

    2018-04-01

    Mid-infrared spectroscopy offers supreme sensitivity for the detection of trace gases, solids and liquids based on tell-tale vibrational bands specific to this spectral region. Here, we present a new platform for mid-infrared dual-comb Fourier-transform spectroscopy based on a pair of ultra-broadband subharmonic optical parametric oscillators pumped by two phase-locked thulium-fibre combs. Our system provides fast (7 ms for a single interferogram), moving-parts-free, simultaneous acquisition of 350,000 spectral data points, spaced by a 115 MHz intermodal interval over the 3.1-5.5 µm spectral range. Parallel detection of 22 trace molecular species in a gas mixture, including isotopologues containing isotopes such as 13C, 18O, 17O, 15N, 34S, 33S and deuterium, with part-per-billion sensitivity and sub-Doppler resolution is demonstrated. The technique also features absolute optical frequency referencing to an atomic clock, a high degree of mutual coherence between the two mid-infrared combs with a relative comb-tooth linewidth of 25 mHz, coherent averaging and feasibility for kilohertz-scale spectral resolution.

  14. Prediction error and trace dominance determine the fate of fear memories after post-training manipulations

    PubMed Central

    Alfei, Joaquín M.; Ferrer Monti, Roque I.; Molina, Victor A.; Bueno, Adrián M.

    2015-01-01

    Different mnemonic outcomes have been observed when associative memories are reactivated by CS exposure and followed by amnestics. These outcomes include mere retrieval, destabilization–reconsolidation, a transitional period (which is insensitive to amnestics), and extinction learning. However, little is known about the interaction between initial learning conditions and these outcomes during a reinforced or nonreinforced reactivation. Here we systematically combined temporally specific memories with different reactivation parameters to observe whether these four outcomes are determined by the conditions established during training. First, we validated two training regimens with different temporal expectations about US arrival. Then, using Midazolam (MDZ) as an amnestic agent, fear memories in both learning conditions were submitted to retraining either under identical or different parameters to the original training. Destabilization (i.e., susceptibly to MDZ) occurred when reactivation was reinforced, provided the occurrence of a temporal prediction error about US arrival. In subsequent experiments, both treatments were systematically reactivated by nonreinforced context exposure of different lengths, which allowed to explore the interaction between training and reactivation lengths. These results suggest that temporal prediction error and trace dominance determine the extent to which reactivation produces the different outcomes. PMID:26179232

  15. Determination of perfluorocompounds in popcorn packaging by pressurised liquid extraction and ultra-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Martínez-Moral, María Pilar; Tena, María Teresa

    2012-11-15

    The development and characterisation of a method based on reverse-phase ultra-performance liquid chromatography (UPLC) coupled to a quadrupole-time of flight mass spectrometer (Q-TOF-MS) with negative electrospray ionisation (ESI) to determine perfluorinated compounds (PFCs) in packaging is presented in this paper. Analytes were quantitatively recovered from packaging with methanol in only one PLE cycle of 6 min at 100 °C. The UPLC allowed the successful separation of the studied PFCs in less than 4 min. The whole method presented good precision, with RSDs below 8%, LODs from 0.6 to 16 ng g(-1); and excellent recovery values, around 100% in all cases, were achieved. The PLE-UPLC-MS method was applied to the analysis of popcorn packaging for microwave cooking. Besides the most commonly studied PFCs: PFOA and PFOS, the presence of other perfluorocarboxylic acids (PFCAs) in popcorn packaging is evidenced in this work. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Ultra-performance liquid chromatography-tandem mass spectrometry for the determination of atypical antipsychotics and some metabolites in in vitro samples.

    PubMed

    Li, Kun-Yan; Zhou, Yan-Gang; Ren, Hua-Yi; Wang, Feng; Zhang, Bi-Kui; Li, Huan-De

    2007-05-01

    The ultra-performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-ESI-MS/MS) method has been developed to perform the determination of quetiapine, perospirone, aripiprazole and quetiapine sulfoxide in in vitro samples in less than 3 min. The UPLC separation was carried out using an Acquity UPLC BEH C18 column (100 mm x 2.1mm i.d., 1.7 microm particle size) that provided high efficiency and resolution in combination with high linear velocities. The UPLC system was coupled to a Waters Micromass Quattro Premier XE tandem quadrupole mass spectrometer. This system permits high-speed data acquisition without peak intensity degradation, and produces sharp and narrow chromatographic peaks (w(h) about 2.5s) of compounds. The determination was performed in multiple reaction monitoring (MRM) mode. The quantification parameters of the developed method were established, obtaining instrumental LODs lower than 0.005 microg/l and a repeatability at a low concentration level lower than 10% CV (n=10). Finally, the method was successfully applied to the analysis of atypical antipsychotics and some metabolites in in vitro samples.

  17. Distribution of trace elements in the coastal sea sediments of Maslinica Bay, Croatia

    NASA Astrophysics Data System (ADS)

    Mikulic, Nenad; Orescanin, Visnja; Elez, Loris; Pavicic, Ljiljana; Pezelj, Durdica; Lovrencic, Ivanka; Lulic, Stipe

    2008-02-01

    Spatial distributions of trace elements in the coastal sea sediments and water of Maslinica Bay (Southern Adriatic), Croatia and possible changes in marine flora and foraminifera communities due to pollution were investigated. Macro, micro and trace elements’ distributions in five granulometric fractions were determined for each sediment sample. Bulk sediment samples were also subjected to leaching tests. Elemental concentrations in sediments, sediment extracts and seawater were measured by source excited energy dispersive X-ray fluorescence (EDXRF). Concentrations of the elements Cr, Cu, Zn, and Pb in bulk sediment samples taken in the Maslinica Bay were from 2.1 to over six times enriched when compared with the background level determined for coarse grained carbonate sediments. A low degree of trace elements leaching determined for bulk sediments pointed to strong bonding of trace elements to sediment mineral phases. The analyses of marine flora pointed to higher eutrophication, which disturbs the balance between communities and natural habitats.

  18. Geodynamic environments of ultra-slow spreading

    NASA Astrophysics Data System (ADS)

    Kokhan, Andrey; Dubinin, Evgeny

    2015-04-01

    Ultra-slow spreading is clearly distinguished as an outstanding type of crustal accretion by recent studies. Spreading ridges with ultra-slow velocities of extension are studied rather well. But ultra-slow spreading is characteristic feature of not only spreading ridges, it can be observed also on convergent and transform plate boundaries. Ultra-slow spreading is observed now or could have been observed in the past in the following geodynamic environments on divergent plate boundaries: 1. On spreading ridges with ultra-slow spreading, both modern (f.e. Gakkel, South-West Indian, Aden spreading center) and ceased (Labrador spreading center, Aegir ridge); 2. During transition from continental rifting to early stages of oceanic spreading (all spreading ridges during incipient stages of their formation); 3. During incipient stages of formation of spreading ridges on oceanic crust as a result of ridge jumps and reorganization of plate boundaries (f.e. Mathematicians rise and East Pacific rise); 4. During propagation of spreading ridge into the continental crust under influence of hotspot (Aden spreading center and Afar triple junction), under presence of strike-slip faults preceding propagation (possibly, rift zone of California Bay). Ultra-slow spreading is observed now or could have been observed in the past in the following geodynamic environments on transform plate boundaries: 1. In transit zones between two "typical" spreading ridges (f.e. Knipovich ridge); 2. In semi strike-slip/extension zones on the oceanic crust (f.e. American-Antarctic ridge); 3. In the zones of local extension in regional strike-slip areas in pull-apart basins along transform boundaries (Cayman trough, pull-apart basins of the southern border of Scotia plate). Ultra-slow spreading is observed now or could have been observed in the past in the following geodynamic environments on convergent plate boundaries: 1. During back-arc rifting on the stage of transition into back-arc spreading (central

  19. Optical bandgap of single- and multi-layered amorphous germanium ultra-thin films

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

    Liu, Pei; Zaslavsky, Alexander; Longo, Paolo

    2016-01-07

    Accurate optical methods are required to determine the energy bandgap of amorphous semiconductors and elucidate the role of quantum confinement in nanometer-scale, ultra-thin absorbing layers. Here, we provide a critical comparison between well-established methods that are generally employed to determine the optical bandgap of thin-film amorphous semiconductors, starting from normal-incidence reflectance and transmittance measurements. First, we demonstrate that a more accurate estimate of the optical bandgap can be achieved by using a multiple-reflection interference model. We show that this model generates more reliable results compared to the widely accepted single-pass absorption method. Second, we compare two most representative methods (Taucmore » and Cody plots) that are extensively used to determine the optical bandgap of thin-film amorphous semiconductors starting from the extracted absorption coefficient. Analysis of the experimental absorption data acquired for ultra-thin amorphous germanium (a-Ge) layers demonstrates that the Cody model is able to provide a less ambiguous energy bandgap value. Finally, we apply our proposed method to experimentally determine the optical bandgap of a-Ge/SiO{sub 2} superlattices with single and multiple a-Ge layers down to 2 nm thickness.« less

  20. Optical Physics Study of Laser Interactions with Solids for Ultra-Trace Materials Analysis Using RIS. Phase 1.

    DTIC Science & Technology

    1987-04-24

    eliminated. Averaging the mass spectra from only 500 laser shots (50 seconds with this system) resulted in a detection limit of r15 ppb. The...resolution. Fluctuations in laser pulse energy from shot to shot appear as noise in the interleaved data, but averaging of several such traces gives a good...ranging from 0to 120 ix Wm- 2. quantity of material volatilized was proportional to the number of lase shots . A simple time-of-flight mass spectrometer was

  1. Characterisation of a natural quartz crystal as a reference material for microanalytical determination of Ti, Al, Li, Fe, Mn, Ga and Ge

    USGS Publications Warehouse

    Audetat, Andreas; Garbe-Schonberg, Dieter; Kronz, Andreas; Pettke, Thomas; Rusk, Brian G.; Donovan, John J.; Lowers, Heather

    2015-01-01

    A natural smoky quartz crystal from Shandong province, China, was characterised by laser ablation ICP-MS, electron probe microanalysis (EPMA) and solution ICP-MS to determine the concentration of twenty-four trace and ultra trace elements. Our main focus was on Ti quantification because of the increased use of this element for titanium-in-quartz (TitaniQ) thermobarometry. Pieces of a uniform growth zone of 9 mm thickness within the quartz crystal were analysed in four different LA-ICP-MS laboratories, three EPMA laboratories and one solution-ICP-MS laboratory. The results reveal reproducible concentrations of Ti (57 ± 4 μg g-1), Al (154 ± 15 μg g-1), Li (30 ± 2 μg g-1), Fe (2.2 ± 0.3 μg g-1), Mn (0.34 ± 0.04 μg g-1), Ge (1.7 ± 0.2 μg g-1) and Ga (0.020 ± 0.002 μg g-1) and detectable, but less reproducible, concentrations of Be, B, Na, Cu, Zr, Sn and Pb. Concentrations of K, Ca, Sr, Mo, Ag, Sb, Ba and Au were below the limits of detection of all three techniques. The uncertainties on the average concentration determinations by multiple techniques and laboratories for Ti, Al, Li, Fe, Mn, Ga and Ge are low; hence, this quartz can serve as a reference material or a secondary reference material for microanalytical applications involving the quantification of trace elements in quartz.

  2. Suitability of ultra-high performance liquid chromatography for the determination of fat-soluble nutritional status (vitamins A, E, D, and individual carotenoids).

    PubMed

    Granado-Lorencio, F; Herrero-Barbudo, C; Blanco-Navarro, I; Pérez-Sacristán, B

    2010-06-01

    Our aim was to assess the suitability of ultra-high performance liquid chromatography (UHPLC) for the simultaneous determination of biomarkers of vitamins A (retinol, retinyl esters), E (alpha- and gamma-tocopherol), D (25-OH-vitamin D), and the major carotenoids in human serum to be used in clinical practice. UHPLC analysis was performed on HSS T3 column (2.1 x 100 mm; 1.8 microm) using gradient elution and UV-VIS detection. The system allows the simultaneous determination of retinol, retinyl palmitate, 25-OH-vitamin D, alpha- and gamma-tocopherol, lutein plus zeaxanthin, alpha-carotene, beta-carotene, alpha- and beta-cryptoxanthin and lycopene. The method showed a good linearity over the physiological range with an adequate accuracy in samples from quality control programs. Suitability of the method in clinical practice was tested by analyzing samples (n = 286) from patients. In conclusion, UHPLC constitutes a reliable approach for nutrient/biomarker profiling allowing the rapid, simultaneous and low-cost determination of vitamins A, E, and D (including vitamers and ester forms) and the major carotenoids in clinical practice.

  3. Flow injection determination of aluminium by spectrofluorimetric detection after complexation with N-o-vanillidine-2-amino-p-cresol: the application to natural waters.

    PubMed

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

    2008-03-17

    An on-line flow injection spectrofluorimetric method for the direct determination of aluminium in water samples is described. The method is based on the reaction of aluminium with N-o-vanillidine-2-amino-p-cresol (OVAC) in acidic medium at pH 4.0 to form a water-soluble complex. The excitation and emission wavelengths were 423.0 and 553.0nm, respectively, at which the OVAC-Al complex gave the maximum fluorescence intensity at pH 4.0 in a 50% methanol-50% water medium at 50 degrees C. An interference from fluoride ions was minimised by the addition of Be(2+). Other ions were found not to interfere at the concentrations likely to be found in natural waters. The proposed methods were validated in terms of linearity, repeatability, detection limit, accuracy and selectivity. Under these conditions, the calibration was linear up to 1000microgL(-1) (r=0.999). The limit of detection (3sigma) for the determination of Al(III) was 0.057microgL(-1) and the precision for multiple determinations of 3ngmL(-1) Al(III) prepared in ultra-pure water was found to be 0.62% (n=10). The Schiff base ligand could be used to determine ultra-trace aluminium from natural waters. Analysis of environmental certified reference materials showed good agreement with the certified values. The procedure was found to be equally applicable to both freshwater and saline solutions, including seawater.

  4. Atmospheric trace metals measured at a regional background site (Welgegund) in South Africa

    NASA Astrophysics Data System (ADS)

    Venter, Andrew D.; van Zyl, Pieter G.; Beukes, Johan P.; Josipovic, Micky; Hendriks, Johan; Vakkari, Ville; Laakso, Lauri

    2017-03-01

    Atmospheric trace metals can cause a variety of health-related and environmental problems. Only a few studies on atmospheric trace metal concentrations have been conducted in South Africa. Therefore the aim of this study was to determine trace metal concentrations in aerosols collected at a regional background site, i.e. Welgegund, South Africa. PM1, PM1-2. 5 and PM2. 5-10 samples were collected for 13 months, and 31 atmospheric trace metal species were detected. Atmospheric iron (Fe) had the highest concentrations in all three size fractions, while calcium (Ca) was the second-most-abundant species. Chromium (Cr) and sodium (Na) concentrations were the third- and fourth-most-abundant species, respectively. The concentrations of the trace metal species in all three size ranges were similar, with the exception of Fe, which had higher concentrations in the PM1 size fraction. With the exception of titanium (Ti), aluminium (Al) and manganese (Mg), 70 % or more of the trace metal species detected were in the smaller size fractions, which indicated the influence of industrial activities. However, the large influence of wind-blown dust was reflected by 30 % or more of trace metals being present in the PM2. 5-10 size fraction. Comparison of trace metals determined at Welgegund to those in the western Bushveld Igneous Complex indicated that at both locations similar species were observed, with Fe being the most abundant. However, concentrations of these trace metal species were significantly higher in the western Bushveld Igneous Complex. Fe concentrations at the Vaal Triangle were similar to levels thereof at Welgegund, while concentrations of species associated with pyrometallurgical smelting were lower. Annual average Ni was 4 times higher, and annual average As was marginally higher than their respective European standard values, which could be attributed to regional influence of pyrometallurgical industries in the western Bushveld Igneous Complex. All three size

  5. Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches.

    PubMed

    Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

    2017-02-15

    A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu 2+ ), cobalt ions (Co 2+ ) and nickel ions (Ni 2+ ) mixture was 0.10μgL -1 , 0.15μgL -1 and 0.13μgL -1 , respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Trace gas emissions from chaparral and boreal forest fires

    NASA Technical Reports Server (NTRS)

    Cofer, Wesley R., III; Levine, Joel S.; Sebacher, Daniel I.; Winstead, Edward L.; Riggan, Philip J.; Stocks, Brian J.; Brass, James A.; Ambrosia, Vincent G.

    1989-01-01

    Using smoke samples collected during low-level helicopter flights, the mixing ratios of CO2, CO, CH4, total nonmethane hydrocarbons, H2, and N2O over burning chaparral in southern California and over a burning boreal forest site in northern Ontario, Canada, were determined. Carbon dioxide-normalized emission ratios were determined for each trace gas for conditions of flaming, mixed, and smoldering combustion. The emission ratios for these trace gases were found to be highest for the smoldering combustion, generally thought to be the least efficient combustion stage. However, high emission ratios for these gases could be also produced during very vigorous flaming combustion.

  7. Analyzing Flash Flood Data in an Ultra-Urban Region

    NASA Astrophysics Data System (ADS)

    Smith, B. K.; Rodriguez, S.

    2016-12-01

    New York City is an ultra-urban region, with combined sewers and buried stream channels. Traditional flood studies rely on the presence of stream gages to detect flood stage and discharge, but ultra-urban regions frequently lack the surface stream channels and gages necessary for this approach. In this study we aggregate multiple non-traditional data for detecting flash flood events. These data including phone call reports, city records, and, for one particular flood event, news reports and social media reports. These data are compared with high-resolution bias-corrected radar rainfall fields to study flash flood events in New York City. We seek to determine if these non-traditional data will allow for a comprehensive study of rainfall-runoff relationships in New York City. We also seek to map warm season rainfall heterogeneities in the city and to compare them to spatial distribution of reported flood occurrence.

  8. Multi-component determination and chemometric analysis of Paris polyphylla by ultra high performance liquid chromatography with photodiode array detection.

    PubMed

    Chen, Pei; Jin, Hong-Yu; Sun, Lei; Ma, Shuang-Cheng

    2016-09-01

    Multi-source analysis of traditional Chinese medicine is key to ensuring its safety and efficacy. Compared with traditional experimental differentiation, chemometric analysis is a simpler strategy to identify traditional Chinese medicines. Multi-component analysis plays an increasingly vital role in the quality control of traditional Chinese medicines. A novel strategy, based on chemometric analysis and quantitative analysis of multiple components, was proposed to easily and effectively control the quality of traditional Chinese medicines such as Chonglou. Ultra high performance liquid chromatography was more convenient and efficient. Five species of Chonglou were distinguished by chemometric analysis and nine saponins, including Chonglou saponins I, II, V, VI, VII, D, and H, as well as dioscin and gracillin, were determined in 18 min. The method is feasible and credible, and enables to improve quality control of traditional Chinese medicines and natural products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Neuroprotective Effects of Co-UltraPEALut on Secondary Inflammatory Process and Autophagy Involved in Traumatic Brain Injury.

    PubMed

    Cordaro, Marika; Impellizzeri, Daniela; Paterniti, Irene; Bruschetta, Giuseppe; Siracusa, Rosalba; De Stefano, Daniela; Cuzzocrea, Salvatore; Esposito, Emanuela

    2016-01-01

    Traumatic brain injury (TBI) initiates a neuroinflammatory cascade that contributes to neuronal damage and behavioral impairment. In the present study, we performed a widely used model of TBI to determine the neuroprotective propriety of palmitoylethanolamide (PEA) and the antioxidant effect of a flavonoid luteolin (Lut), given as a co-ultramicronized compound Co-ultraPEALut. We demonstrated that the treatment with Co-ultraPEALut resulted in a significant improvement of motor and cognitive recovery after controlled cortical impact, as well as markedly reducing lesion volumes. Moreover, our results revealed the ability of Co-ultraPEALut to reduce brain trauma through modulation of nuclear factor-κB activation. In addition, treatment with Co-ultraPEALut significantly enhanced the post-TBI expression of the neuroprotective neurotrophins glial cell line-derived neurotrophic factor compared with vehicle. Co-ultraPEALut at the dose of 1 mg/kg also modulated apoptosis, the release of cytokine and reactive oxygen species, the activation of chymase, tryptase, and nitrotyrosine, and inhibited autophagy. Thus, our data demonstrated that Co-ultraPEALut at a lower dose compared with PEA alone can exert neuroprotective effects and the combination of both could improve their ability to counteract the neurodegeneration and neuroinflammation induced by TBI.

  10. Co-detection: ultra-reliable nanoparticle-based electrical detection of biomolecules in the presence of large background interference.

    PubMed

    Liu, Yang; Gu, Ming; Alocilja, Evangelyn C; Chakrabartty, Shantanu

    2010-11-15

    An ultra-reliable technique for detecting trace quantities of biomolecules is reported. The technique called "co-detection" exploits the non-linear redundancy amongst synthetically patterned biomolecular logic circuits for deciphering the presence or absence of target biomolecules in a sample. In this paper, we verify the "co-detection" principle on gold-nanoparticle-based conductimetric soft-logic circuits which use a silver-enhancement technique for signal amplification. Using co-detection, we have been able to demonstrate a great improvement in the reliability of detecting mouse IgG at concentration levels that are 10(5) lower than the concentration of rabbit IgG which serves as background interference. Copyright © 2010 Elsevier B.V. All rights reserved.

  11. Trace elements in seminal plasma of men from infertile couples.

    PubMed

    Guzikowski, Wojciech; Szynkowska, Małgorzata I; Motak-Pochrzęst, Hanna; Pawlaczyk, Aleksandra; Sypniewski, Stanisław

    2015-06-19

    An analysis of lead, zinc, cadmium and other trace elements in semen of men from infertile couples was performed to determine the association between abnormal semen parameters and enviromental or occupational exposure to some trace metals. Presence of manganese, cobalt, nickel, copper, zinc, molybdenum, cadmium, tin and lead was measured in seminal plasma of 34 men from infertile couples using spectrometry with time-of-flight analysis. Correlations among sperm parameters and trace metals were determined using cluster analysis and Pearson's correlation coefficient. Abnormally high concentrations of lead, cadmium, zinc and cobalt were found in 23 seminal plasma of men from infertile couples. The most consistent evidence was determined for an association between high cadmium concentration in seminal plasma and sperm count, motility and morphology below reference limits (p < 0.01). A correlation of significantly increased tin level and reduced sperm count in semen of men with limited fertility potential was observed (p = 0.04). In our study we observed a correlation of tin level with sperm count in semen of men with limited fertility potential.

  12. A method for establishing constraints on galactic magnetic field models using ultra high energy cosmic rays and results from the data of the Pierre Auger Observatory

    NASA Astrophysics Data System (ADS)

    Sutherland, Michael Stephen

    2010-12-01

    The Galactic magnetic field is poorly understood. Essentially the only reliable measurements of its properties are the local orientation and field strength. Its behavior at galactic scales is unknown. Historically, magnetic field measurements have been performed using radio astronomy techniques which are sensitive to certain regions of the Galaxy and rely upon models of the distribution of gas and dust within the disk. However, the deflection of trajectories of ultra high energy cosmic rays arriving from extragalactic sources depends only on the properties of the magnetic field. In this work, a method is developed for determining acceptable global models of the Galactic magnetic field by backtracking cosmic rays through the field model. This method constrains the parameter space of magnetic field models by comparing a test statistic between backtracked cosmic rays and isotropic expectations for assumed cosmic ray source and composition hypotheses. Constraints on Galactic magnetic field models are established using data from the southern site of the Pierre Auger Observatory under various source distribution and cosmic ray composition hypotheses. Field models possessing structure similar to the stellar spiral arms are found to be inconsistent with hypotheses of an iron cosmic ray composition and sources selected from catalogs tracing the local matter distribution in the universe. These field models are consistent with hypothesis combinations of proton composition and sources tracing the local matter distribution. In particular, strong constraints are found on the parameter space of bisymmetric magnetic field models scanned under hypotheses of proton composition and sources selected from the 2MRS-VS, Swift 39-month, and VCV catalogs. Assuming that the Galactic magnetic field is well-described by a bisymmetric model under these hypotheses, the magnetic field strength near the Sun is less than 3-4 muG and magnetic pitch angle is less than -8°. These results comprise

  13. Ultra-Deep Drilling Cost Reduction; Design and Fabrication of an Ultra-Deep Drilling Simulator (UDS)

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

    Lindstrom, Jason

    2010-01-31

    Ultra-deep drilling, below about 20,000 ft (6,096 m), is extremely expensive and limits the recovery of hydrocarbons at these depths. Unfortunately, rock breakage and cuttings removal under these conditions is not understood. To better understand and thus reduce cost at these conditions an ultra-deep single cutter drilling simulator (UDS) capable of drill cutter and mud tests to sustained pressure and temperature of 30,000 psi (207 MPa) and 482 °F (250 °C), respectively, was designed and manufactured at TerraTek, a Schlumberger company, in cooperation with the Department of Energy’s National Energy Technology Laboratory. UDS testing under ultra-deep drilling conditions offers anmore » economical alternative to high day rates and can prove or disprove the viability of a particular drilling technique or fluid to provide opportunity for future domestic energy needs.« less

  14. Development and ultra-structure of an ultra-thin silicone epidermis of bioengineered alternative tissue.

    PubMed

    Wessels, Quenton; Pretorius, Etheresia

    2015-08-01

    Burn wound care today has a primary objective of temporary or permanent wound closure. Commercially available engineered alternative tissues have become a valuable adjunct to the treatment of burn injuries. Their constituents can be biological, alloplastic or a combination of both. Here the authors describe the aspects of the development of a siloxane epidermis for a collagen-glycosaminoglycan and for nylon-based artificial skin replacement products. A method to fabricate an ultra-thin epidermal equivalent is described. Pores, to allow the escape of wound exudate, were punched and a tri-filament nylon mesh or collagen scaffold was imbedded and silicone polymerisation followed at 120°C for 5 minutes. The ultra-structure of these bilaminates was assessed through scanning electron microscopy. An ultra-thin biomedical grade siloxane film was reliably created through precision coating on a pre-treated polyethylene terephthalate carrier. © 2013 The Authors. International Wound Journal © 2013 Medicalhelplines.com Inc and John Wiley & Sons Ltd.

  15. A low-cost, ultra-fast and ultra-low noise preamplifier for silicon avalanche photodiodes

    NASA Astrophysics Data System (ADS)

    Gasmi, Khaled

    2018-02-01

    An ultra-fast and ultra-low noise preamplifier for amplifying the fast and weak electrical signals generated by silicon avalanche photodiodes has been designed and developed. It is characterized by its simplicity, compactness, reliability and low cost of construction. A very wide bandwidth of 300 MHz, a very good linearity from 1 kHz to 280 MHz, an ultra-low noise level at the input of only 1.7 nV Hz-1/2 and a very good stability are its key features. The compact size (70 mm  ×  90 mm) and light weight (45 g), as well as its excellent characteristics, make this preamplifier very competitive compared to any commercial preamplifier. The preamplifier, which is a main part of the detection system of a homemade laser remote sensing system, has been successfully tested. In addition, it is versatile and can be used in any optical detection system requiring high speed and very low noise electronics.

  16. Spectrophotometric determination of trace carbaryl in water and grain samples by inhibition of the rhodamine-B oxidation.

    PubMed

    Gupta, Nirja; Pillai, Ajai Kumar; Parmar, Prachi

    2015-03-15

    A novel, sensitive, selective and simple kinetic spectrophotometric method has been developed for determination of trace levels of carbaryl based on its inhibitory effect on the oxidation of rhodamine-B by chlorine and bromine released from reaction of potassium bromate with hydrochloric acid in micellar medium. A linear relationship was observed between the inhibitory effect and the concentration of the compound. The absorbance was monitored at the maximum wavelength of 555 nm. The effect of different parameters such as pH, temperature and concentration of rhodamine-B, potassium bromate and surfactant on the reaction were investigated and optimum conditions were established. Under the selected experimental conditions, carbaryl was determined in the range of 0.04-0.4 μg mL(-1). Sandell's sensitivity and molar absorptivity were found to be 0.00055 μg cm(-2) and 3.658×10(5) L mol(-1) cm(-1) respectively. The proposed method was applied satisfactorily for the determination of carbaryl in water and different grain samples. The results were compared with those obtained by reference method and were found to be in agreement. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Review on the progress of ultra-precision machining technologies

    NASA Astrophysics Data System (ADS)

    Yuan, Julong; Lyu, Binghai; Hang, Wei; Deng, Qianfa

    2017-06-01

    Ultra-precision machining technologies are the essential methods, to obtain the highest form accuracy and surface quality. As more research findings are published, such technologies now involve complicated systems engineering and been widely used in the production of components in various aerospace, national defense, optics, mechanics, electronics, and other high-tech applications. The conception, applications and history of ultra-precision machining are introduced in this article, and the developments of ultra-precision machining technologies, especially ultra-precision grinding, ultra-precision cutting and polishing are also reviewed. The current state and problems of this field in China are analyzed. Finally, the development trends of this field and the coping strategies employed in China to keep up with the trends are discussed.

  18. Processed and ultra-processed foods are associated with lower-quality nutrient profiles in children from Colombia.

    PubMed

    Cornwell, Brittany; Villamor, Eduardo; Mora-Plazas, Mercedes; Marin, Constanza; Monteiro, Carlos A; Baylin, Ana

    2018-01-01

    To determine if processed and ultra-processed foods consumed by children in Colombia are associated with lower-quality nutrition profiles than less processed foods. We obtained information on sociodemographic and anthropometric variables and dietary information through dietary records and 24 h recalls from a convenience sample of the Bogotá School Children Cohort. Foods were classified into three categories: (i) unprocessed and minimally processed foods, (ii) processed culinary ingredients and (iii) processed and ultra-processed foods. We also examined the combination of unprocessed foods and processed culinary ingredients. Representative sample of children from low- to middle-income families in Bogotá, Colombia. Children aged 5-12 years in 2011 Bogotá School Children Cohort. We found that processed and ultra-processed foods are of lower dietary quality in general. Nutrients that were lower in processed and ultra-processed foods following adjustment for total energy intake included: n-3 PUFA, vitamins A, B12, C and E, Ca and Zn. Nutrients that were higher in energy-adjusted processed and ultra-processed foods compared with unprocessed foods included: Na, sugar and trans-fatty acids, although we also found that some healthy nutrients, including folate and Fe, were higher in processed and ultra-processed foods compared with unprocessed and minimally processed foods. Processed and ultra-processed foods generally have unhealthy nutrition profiles. Our findings suggest the categorization of foods based on processing characteristics is promising for understanding the influence of food processing on children's dietary quality. More studies accounting for the type and degree of food processing are needed.

  19. Real-time trace ambient ammonia monitor for haze prevention

    NASA Astrophysics Data System (ADS)

    Nishimura, Katsumi; Sakaguchi, Yuhei; Crosson, Eric; Wahl, Edward; Rella, Chris

    2007-05-01

    In photolithography, haze prevention is of critical importance to integrated circuit chip manufacturers. Numerous studies have established that the presence of ammonia in the photolithography tool can cause haze to form on optical surfaces resulting in permanent damage to costly deep ultra-violet optics. Ammonia is emitted into wafer fab air by various semiconductor processes including coating steps in the track and CMP. The workers in the clean room also emit a significant amount of ammonia. Chemical filters are typically used to remove airborne contamination from critical locations but their lifetime and coverage cannot offer complete protection. Therefore, constant or periodic monitoring of airborne ammonia at parts-per-trillion (ppt) levels is critical to insure the integrity of the lithography process. Real time monitoring can insure that an accidental ammonia release in the clean room is detected before any optics is damaged. We have developed a transportable, highly accurate, highly specific, real-time trace gas monitor that detects ammonia using Cavity Ring-Down Spectroscopy (CRDS). The trace gas monitor requires no calibration gas standards, and can measure ammonia with 200 ppt sensitivity in five minutes with little or no baseline drift. In addition, the high spectral resolution of CRDS makes the analyzer less susceptible to interference from other gases when compared to other detection methods. In this paper we describe the monitor, focus on its performance, discuss the results of a careful comparison with ion chromatography (IC), and present field data measured inside the aligner and the reticule stocker at a semiconductor fab.

  20. Simultaneous determination of 30 ginsenosides in Panax ginseng preparations using ultra performance liquid chromatography

    PubMed Central

    Park, Hee-Won; In, Gyo; Han, Sung-Tai; Lee, Myoung-Woo; Kim, So-Young; Kim, Kyung-Tack; Cho, Byung-Goo; Han, Gyeong-Ho; Chang, Il-Moo

    2013-01-01

    A quick and simple method for simultaneous determination of the 30 ginsenosides (ginsenoside Ro, Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, 20(S)-Rg2, 20(R)-Rg2, 20(S)-Rg3, 20(R)-Rg3, 20(S)-Rh1, 20(S)-Rh2, 20(R)-Rh2, F1, F2, F4, Ra1, Rg6, Rh4, Rk3, Rg5, Rk1, Rb3, Rk2, Rh3, compound Y, compound K, and notoginsenoside R1) in Panax ginseng preparations was developed and validated by an ultra performance liquid chromatography photo diode array detector. The separation of the 30 ginsenosides was efficiently undertaken on the Acquity BEH C-18 column with gradient elution with phosphoric acids. Especially the chromatogram of the ginsenoside Ro was dramatically enhanced by adding phosphoric acid. Under optimized conditions, the detection limits were 0.4 to 1.7 mg/L and the calibration curves of the peak areas for the 30 ginsenosides were linear over three orders of magnitude with a correlation coefficients greater than 0.999. The accuracy of the method was tested by a recovery measurement of the spiked samples which yielded good results of 89% to 118%. From these overall results, the proposed method may be helpful in the development and quality of P. ginseng preparations because of its wide range of applications due to the simultaneous analysis of many kinds of ginsenosides. PMID:24235860

  1. A fast ultrasound-assisted extraction procedure for trace elements determination in hair samples by ICP-MS for forensic analysis.

    PubMed

    Batista, Bruno Lemos; Rodrigues, Jairo Lisboa; Souza, Vanessa Cristina de Oliveira; Barbosa, Fernando

    2009-11-20

    An ultrasound-assisted extraction method is proposed for the determination of trace elements in hair samples by inductively coupled plasma-mass spectrometry (ICP-MS) for forensic investigation. Prior to analysis, 25mg of hair samples were accurately weighed into (15 mL) conical tubes. Then, 2 mL of 20% HNO(3) is added to the samples, sonicated at 2 min (50W, 100% amplitude), and then further diluted to 10 mL with Milli-Q water. Resulted diluted slurries are centrifuged and the analytes are directly determined in the supernatant. Calibrations against aqueous solutions were carried out with rhodium as internal standard. The method was successfully applied for the extraction of Al, As, Ba, Be, Cd, Co, Cr, Cu, Mn, Pb, Tl, U, V and Zn with a method detection limit (3s, n=20) of 0.1, 0.4, 0.2, 0.09, 0.08, 0.04, 0.1, 2.9, 1.0, 0.9, 0.04, 0.05, 0.1 and 4.2 ng/g, respectively. Method accuracy is traceable to Certified Reference Materials (CRMs) 85 and 86 human hair from the International Atomic Energy Agency (IAEA). Additional validation data are provided based on the analysis of hair samples from the trace elements intercomparison program operated by the Institut National de Sante' Publique du Quebec, Canada. The proposed method is very simple and can be applied for forensic purposes with the elimination of sample digestion step prior to analysis. Then, a considerable improvement in the sample throughput is archived with the use of the proposed method.

  2. Determination of trace level bromate and perchlorate in drinking water by ion chromatography with an evaporative preconcentration technique.

    PubMed

    Liu, Yongjian; Mou, Shifen; Heberling, Shawn

    2002-05-17

    A simple sample preconcentration technique employing microwave-based evaporation for the determination of trace level bromate and perchlorate in drinking water with ion chromatography is presented. With a hydrophilic anion-exchange column and a sodium hydroxide eluent in linear gradient, bromate and perchlorate can be determined in one injection within 35 min. Prior to ion chromatographic analysis, the drinking water sample was treated with an OnGuard-Ag cartridge to remove the superfluous chloride and concentrated 20-fold using a PTFE beaker in a domestic microwave oven for 15 min. The recoveries of the anions ranged from 94.6% for NO2- to 105.2% for F-. The detection limits for bromate, perchlorate, iodate and chlorate were 0.1, 0.2, 0.1 and 0.2 microg/l, respectively. The developed method is applicable for the quantitation of bromate and perchlorate in drinking water samples.

  3. Trace determination of organophosphate esters in white wine, red wine, and beer samples using dispersive liquid-liquid microextraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Pang, Long; Yang, Huiqiang; Yang, Peijie; Zhang, Hongzhong; Zhao, Jihong

    2017-08-15

    In this study, dispersive liquid-liquid microextraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry was developed for the analysis of five representative organophosphate esters (OPEs) in wine samples. Under optimized conditions, the proposed method resulted in good linearity (R 2 >0.9933) over the range of 0.1-100μgL -1 , with limits of detection (LODs, S/N =3) and quantification (LOQs, S/N =10) in the ranges of 0.48-18.8ngL -1 and 1.58-62.5ngL -1 , respectively. Inter- and intra-assay precisions of RSD% ranged from 3.21% to 6.13% and from 1.69% to 7.63%, respectively. The spiked recoveries of target OPEs from white wine, red wine, and beer samples were in the ranges of 80-122%, 76-120%, and 76-110%, respectively, at two different concentration levels. The total concentrations of five OPEs found in white wine, red wine, and beer samples were in the ranges of 0.29-0.85μgL -1 , 1.00-3.05μgL -1 , and 0.86-1.47μgL -1 , respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples.

    PubMed

    Yang, Xiupei; Jia, Zhihui; Yang, Xiaocui; Li, Gu; Liao, Xiangjun

    2017-03-01

    A cloud point extraction (CPE) method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS) The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I)/diethyldithiocarbamate (DDTC) complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I)/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL -1 Ag + in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL -1 for both Zn 2+ and Cu 2+ , 80 μg·mL -1 for Pb 2+ , 1000 μg·mL -1 for Mn 2+ , and 100 μg·mL -1 for both Cd 2+ and Ni 2+ . The calibration curve was linear in the range of 1-500 ng·mL -1 with a limit of detection (LOD) at 0.3 ng·mL -1 . The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

  5. Consumption of ultra-processed foods predicts diet quality in Canada.

    PubMed

    Moubarac, Jean-Claude; Batal, M; Louzada, M L; Martinez Steele, E; Monteiro, C A

    2017-01-01

    This study describes food consumption patterns in Canada according to the types of food processing using the Nova classification and investigates the association between consumption of ultra-processed foods and the nutrient profile of the diet. Dietary intakes of 33,694 individuals from the 2004 Canadian Community Health Survey aged 2 years and above were analyzed. Food and drinks were classified using Nova into unprocessed or minimally processed foods, processed culinary ingredients, processed foods and ultra-processed foods. Average consumption (total daily energy intake) and relative consumption (% of total energy intake) provided by each of the food groups were calculated. Consumption of ultra-processed foods according to sex, age, education, residential location and relative family revenue was assessed. Mean nutrient content of ultra-processed foods and non-ultra-processed foods were compared, and the average nutrient content of the overall diet across quintiles of dietary share of ultra-processed foods was measured. In 2004, 48% of calories consumed by Canadians came from ultra-processed foods. Consumption of such foods was high amongst all socioeconomic groups, and particularly in children and adolescents. As a group, ultra-processed foods were grossly nutritionally inferior to non-ultra-processed foods. After adjusting for covariates, a significant and positive relationship was found between the dietary share of ultra-processed foods and the content in carbohydrates, free sugars, total and saturated fats and energy density, while an inverse relationship was observed with the dietary content in protein, fiber, vitamins A, C, D, B6 and B12, niacin, thiamine, riboflavin, as well as zinc, iron, magnesium, calcium, phosphorus and potassium. Lowering the dietary share of ultra-processed foods and raising consumption of hand-made meals from unprocessed or minimally processed foods would substantially improve the diet quality of Canadian. Copyright © 2016

  6. Quantitative Analysis of Trace Element Impurity Levels in Some Gem-Quality Diamonds

    NASA Astrophysics Data System (ADS)

    McNeill, J. C.; Klein-Bendavid, O.; Pearson, D. G.; Nowell, G. M.; Ottley, C. J.; Chinn, I.; Malarkey, J.

    2009-05-01

    Perhaps the most important information required to understand the origin of diamonds is the nature of the fluid that they crystallise from. Constraining the identity of the diamond-forming fluid for high purity gem diamonds is hampered by analytical challenges because of the very low analyte levels involved. Here we use a new ultra- low blank 'off-line' laser ablation method coupled to sector-field ICPMS for the quantitative analysis of fluid-poor gem diamonds. Ten diamonds comprised of both E- and P-type parageneses, from the Premier Mine, South Africa, were analysed for trace element abundances. We assume that the elemental signatures arise from low densities of sub-microscopic fluid inclusions that are analogous to the much higher densities of fluid inclusions commonly found within fluid-rich diamonds exhibiting fibrous growth. Repeatability of multiple (>20) blanks yielded consistently low values so that using the current procedure our limits of quantitation (10-ã blank) are <1pg for most trace elements, except for Sr, Zr, Ba, from 2-9pg and Pb ~30pg. Trace element patterns of the Premier diamond suite show enrichment of LREE over HREE. Abundances broadly decrease with increasing elemental compatibility. As a suite the chondrite normalised diamond patterns show negative Sr, Zr, Ti and Y anomalies and positive U, and Pb anomalies. All sample abundances are very depleted relative to chondrites (0.1 to 0.001X ch). HREE range from 0.1 to 1ppb as do Y, Nb, Cs. Other lighter elements vary from 2-30ppb. Pb reaches several ppb and Ti ranges from ppb values up to 2ppm. No significant difference were observed between the trace element systematics of the eclogitic and peridotitic diamonds. Overall, these initial data have inter-element fractionation patterns similar to those evident from fluid-rich fibrous diamonds and can be sued to infer that both types of diamond-forming fluids share a common origin.

  7. Is there still a TRACE of trace?

    NASA Astrophysics Data System (ADS)

    McClelland, James; Mirman, Daniel; Holt, Lori

    2003-04-01

    According to the TRACE model [McClelland and Elman, Cogn. Psychol. 18, 1-86 (1986)], speech recognition is an interactive activation process involving the integrated use of top-down (lexical) and bottom-up (acoustic) information. Although it is widely accepted that there are lexical influences on speech perception, there has been a disagreement over their exact nature. Two contested predictions of TRACE are that (a) lexical influences should delay or inhibit recognition of phonemes not consistent with lexical information and (b) a lexical influence on the identification of one phoneme can trigger compensation for co-articulation, affecting the identification of other phonemes. Others [Norris, McQueen, and Cutler, BBS 23, 299-370 (2000)] have argued that the predicted effects do not occur, taking this to support an alternative to the TRACE model in which lexical influences do not affect perception, but only a post-perceptual identification process. We re-examine the evidence on these points along with the recent finding that lexical information may lead to a lasting adjustment of category boundaries [McQueen, Norris, and Cutler, Psychonomics Abstract 255 (2001)]. Our analysis indicates that the existing evidence is completely consistent with TRACE, and we suggest additional research that will be necessary to resolve unanswered questions.

  8. Cytotoxic effects of ultra-diluted remedies on breast cancer cells.

    PubMed

    Frenkel, Moshe; Mishra, Bal Mukund; Sen, Subrata; Yang, Peiying; Pawlus, Alison; Vence, Luis; Leblanc, Aimee; Cohen, Lorenzo; Banerji, Pratip; Banerji, Prasanta

    2010-02-01

    The use of ultra-diluted natural products in the management of disease and treatment of cancer has generated a lot of interest and controversy. We conducted an in vitro study to determine if products prescribed by a clinic in India have any effect on breast cancer cell lines. We studied four ultra-diluted remedies (Carcinosin, Phytolacca, Conium and Thuja) against two human breast adenocarcinoma cell lines (MCF-7 and MDA-MB-231) and a cell line derived from immortalized normal human mammary epithelial cells (HMLE). The remedies exerted preferential cytotoxic effects against the two breast cancer cell lines, causing cell cycle delay/arrest and apoptosis. These effects were accompanied by altered expression of the cell cycle regulatory proteins, including downregulation of phosphorylated Rb and upregulation of the CDK inhibitor p27, which were likely responsible for the cell cycle delay/arrest as well as induction of the apoptotic cascade that manifested in the activation of caspase 7 and cleavage of PARP in the treated cells. The findings demonstrate biological activity of these natural products when presented at ultra-diluted doses. Further in-depth studies with additional cell lines and animal models are warranted to explore the clinical applicability of these agents.

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

    PubMed

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

    2017-09-01

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

  10. Further demonstration of the VRLA-type UltraBattery under medium-HEV duty and development of the flooded-type UltraBattery for micro-HEV applications

    NASA Astrophysics Data System (ADS)

    Furukawa, J.; Takada, T.; Monma, D.; Lam, L. T.

    The UltraBattery has been invented by the CSIRO Energy Technology in Australia and has been developed and produced by the Furukawa Battery Co., Ltd., Japan. This battery is a hybrid energy storage device which combines a super capacitor and a lead-acid battery in single unit cells, taking the best from both technologies without the need of extra, expensive electronic controls. The capacitor enhances the power and lifespan of the lead-acid battery as it acts as a buffer during high-rate discharging and charging, thus enabling it to provide and absorb charge rapidly during vehicle acceleration and braking. The laboratory results of the prototype valve-regulated UltraBatteries show that the capacity, power, available energy, cold cranking and self-discharge of these batteries have met, or exceeded, all the respective performance targets set for both minimum and maximum power-assist HEVs. The cycling performance of the UltraBatteries under micro-, mild- and full-HEV duties is at least four times longer than that of the state-of-the-art lead-acid batteries. Importantly, the cycling performance of UltraBatteries is proven to be comparable or even better than that of the Ni-MH cells. On the other hand, the field trial of UltraBatteries in the Honda Insight HEV shows that the vehicle has surpassed 170,000 km and the batteries are still in a healthy condition. Furthermore, the UltraBatteries demonstrate very good acceptance of the charge from regenerative braking even at high state-of-charge, e.g., 70% during driving. Therefore, no equalization charge is required for the UltraBatteries during field trial. The HEV powered by UltraBatteries gives slightly higher fuel consumption (cf., 4.16 with 4.05 L/100 km) and CO 2 emissions (cf., 98.8 with 96 g km -1) compared with that by Ni-MH cells. There are no differences in driving experience between the Honda Insight powered by UltraBatteries and by Ni-MH cells. Given such comparable performance, the UltraBattery pack costs

  11. Flow injection on-line displacement/solid phase extraction system coupled with flame atomic absorption spectrometry for selective trace silver determination in water samples.

    PubMed

    Christou, Chrysoula K; Anthemidis, Aristidis N

    2009-04-15

    A novel flow injection (FI) on-line displacement solid phase extraction preconcentration and/or separation method coupled with FAAS in order to minimize interference from other metals was developed for trace silver determination. The proposed method involved the on-line formation and subsequently pre-sorption of lead diethyldithiocarbamate (Pb-DDTC) into a column packed with PTFE-turnings. The preconcentration and/or separation of the Ag(I) took place through a displacement reaction between Ag(I) and Pb(II) of the pre-sorbed Pb-DDTC. Finally, the retained analyte was eluted with isobutyl methyl ketone (IBMK) and delivered directly to nebulizer for measuring. Interference from co-existing ions with lower DDTC complex stability in comparison with Pb-DDTC, was eliminated without need for any masking reagent. With 120 s of preconcentration time at a sample flow rate of 7.6 mL min(-1), an enhancement factor of 110 and a detection limit (3s) of 0.2 microg L(-1) were obtained. The precision (RSD, n=10) was 3.1% at the 10 mug L(-1) level. The developed method was successfully applied to trace silver determination in a variety of environmental water samples and certified reference material.

  12. Ultra High Bypass Integrated System Test

    NASA Image and Video Library

    2015-09-14

    NASA’s Environmentally Responsible Aviation Project, in collaboration with the Federal Aviation Administration (FAA) and Pratt & Whitney, completed testing of an Ultra High Bypass Ratio Turbofan Model in the 9’ x 15’ Low Speed Wind Tunnel at NASA Glenn Research Center. The fan model is representative of the next generation of efficient and quiet Ultra High Bypass Ratio Turbofan Engine designs.

  13. Investigation of Latent Traces Using Infrared Reflectance Hyperspectral Imaging

    NASA Astrophysics Data System (ADS)

    Schubert, Till; Wenzel, Susanne; Roscher, Ribana; Stachniss, Cyrill

    2016-06-01

    The detection of traces is a main task of forensics. Hyperspectral imaging is a potential method from which we expect to capture more fluorescence effects than with common forensic light sources. This paper shows that the use of hyperspectral imaging is suited for the analysis of latent traces and extends the classical concept to the conservation of the crime scene for retrospective laboratory analysis. We examine specimen of blood, semen and saliva traces in several dilution steps, prepared on cardboard substrate. As our key result we successfully make latent traces visible up to dilution factor of 1:8000. We can attribute most of the detectability to interference of electromagnetic light with the water content of the traces in the shortwave infrared region of the spectrum. In a classification task we use several dimensionality reduction methods (PCA and LDA) in combination with a Maximum Likelihood classifier, assuming normally distributed data. Further, we use Random Forest as a competitive approach. The classifiers retrieve the exact positions of labelled trace preparation up to highest dilution and determine posterior probabilities. By modelling the classification task with a Markov Random Field we are able to integrate prior information about the spatial relation of neighboured pixel labels.

  14. Biological application of laser induced breakdown spectroscopy technique for determination of trace elements in hair.

    PubMed

    Emara, Elshaimaa M; Imam, Hisham; Hassan, Mouyed A; Elnaby, Salah H

    2013-12-15

    Analysis of trace elements in mammalian hair has the potential to reveal retrospective information about an individual's nutritional status and exposure. As trace elements are incorporated into the hair during the growth process, longitudinal segments of the hair may reflect the body burden during growth. Using LIBS technique, Na, K, Ca, Mg, Si, Fe, Pb and Zn were detected in a single strand of horse hair. The results obtained through LIBS technique on hair samples were compared with the traditional technique (AAS) on digested acidified solution of the same samples. The effects of the experimental parameters on the emission lines were studied and the local thermodynamic equilibrium (LTE) in produced plasma was investigated. The transient plasma condition was verified at specific time region (1500-2000 ns) in the plasma evolution corresponding to its dynamic expanding characteristic. The relative mass concentrations of Fe and Zn were calculated by setting the concentration of C as the calibration. The information obtained from the trace elements' spectra of horse hair in this study substantiates the potential of hair as a biomarker. © 2013 Elsevier B.V. All rights reserved.

  15. Trace element abundance determinations by Synchrotron X Ray Fluorescence (SXRF) on returned comet nucleus mineral grains

    NASA Technical Reports Server (NTRS)

    Flynn, G. J.; Sutton, S. R.

    1989-01-01

    Trace element analyses were performed on bulk cosmic dust particles by Proton Induced X Ray Emission (PIXE) and Synchrotron X Ray Fluorescence (SXRF). When present at or near chondritic abundances the trace elements K, Ti, Cr, Mn, Cu, Zn, Ga, Ge, Se, and Br are presently detectable by SXRF in particles of 20 micron diameter. Improvements to the SXRF analysis facility at the National Synchrotron Light Source presently underway should increase the range of detectable elements and permit the analysis of smaller samples. In addition the Advanced Photon Source will be commissioned at Argonne National Laboratory in 1995. This 7 to 8 GeV positron storage ring, specifically designed for high-energy undulator and wiggler insertion devices, will be an ideal source for an x ray microprobe with one micron spatial resolution and better than 100 ppb elemental sensitivity for most elements. Thus trace element analysis of individual micron-sized grains should be possible by the time of the comet nucleus sample return mission.

  16. Highly sensitive and selective spectrophotometric method for determination of trace gold in geological samples with 5-(2-hydroxy-5-nitrophenylazo)rhodanine.

    PubMed

    Zaijun, Li; Jiaomai, Pan; Jian, Tang

    2003-02-01

    A excellent sensitive and selective method for spectrophotometric determination of trace gold has been developed, the method is based on the color reaction of gold(III) with new reagent 5-(2-hydroxy-5-nitrophenylazo)rhodanine (HNAR). Under optimal conditions, HNAR reacts with gold(III) to form a 1:5 orange complex, which has an maximum absorption peak at 480 nm. Maximum enhancement of the absorbance of the complex was obtained in the presence of the mixed surfactant of Triton X-100 and CTMAB; the reaction completed rapidly and the absorbance is stable for 5 h at least at 20 degrees C; 0-48 microg L(-1) Au(III) obeyed Beer's law. The apparent molar absorptivity of the complex, Sandell's sensitivity, the limit of quantification, the limit of detection and relative standard deviation were found to be 2.0x10(6) L mol(-1) cm(-1), 0.000,098,483 micro g cm(-2), 1.02 ng mL(-1), 0.35 ng mL(-1) and 1.09%, respectively. The effect of co-existing ions was studied seriously; most metal ions can be tolerated in considerable amounts. Its sensitivity and selectivity are remarkably superior to other reagents in the literature. The proposed method was used successfully to determine trace gold in geological samples. Moreover, the synthesis, characteristics and analytical reaction of HNAR with gold are also described in detail.

  17. The effects of trace element content on pyrite oxidation rates

    NASA Astrophysics Data System (ADS)

    Gregory, D. D.; Lyons, T.; Cliff, J. B.; Perea, D. E.; Johnson, A.; Romaniello, S. J.; Large, R. R.

    2017-12-01

    Pyrite acts as both an important source and sink for many different metals and metalloids in the environment, including many that are toxic. Oxidation of pyrite can release these elements while at the same time producing significant amounts of sulfuric acid. Such issues are common in the vicinity of abandoned mines and smelters, but, as pyrite is a common accessory mineral in many different lithologies, significant pyrite oxidation can occur whenever pyritic rocks are exposed to oxygenated water or the atmosphere. Accelerated exposure to oxygen can occur during deforestation, fracking for petroleum, and construction projects. Geochemical models for pyrite oxidation can help us develop strategies to mitigate these deleterious effects. An important component of these models is an accurate pyrite oxidation rate; however, current pyrite oxidation rates have been determined using relatively pure pyrite. Natural pyrite is rarely pure and has a wide range of trace element concentrations that may affect the oxidation rate. Furthermore, the position of trace elements within the mineral lattice can also affect the oxidation rate. For example, elements such as Ni and Co, which substitute into the pyrite lattice, are thought to stabilize the lattice and thus prevent pyrite oxidation. Alternatively, trace elements that are held within inclusions of other minerals could form a galvanic cell with the surrounding pyrite, thus enhancing pyrite oxidation rates. In this study, we present preliminary analyses from three different pyrite oxidation experiments each using natural pyrite with different trace element compositions. These results show that the pyrite with the highest trace element concentration has approximately an order of magnitude higher oxidation rate compared to the lowest trace element sample. To further elucidate the mechanisms, we employed microanalytical techniques to investigate how the trace elements are held within the pyrite. LA-ICPMS was used to determine the

  18. Multifrequency Ultra-High Resolution Miniature Scanning Microscope Using Microchannel And Solid-State Sensor Technologies And Method For Scanning Samples

    NASA Technical Reports Server (NTRS)

    Wang, Yu (Inventor)

    2006-01-01

    A miniature, ultra-high resolution, and color scanning microscope using microchannel and solid-state technology that does not require focus adjustment. One embodiment includes a source of collimated radiant energy for illuminating a sample, a plurality of narrow angle filters comprising a microchannel structure to permit the passage of only unscattered radiant energy through the microchannels with some portion of the radiant energy entering the microchannels from the sample, a solid-state sensor array attached to the microchannel structure, the microchannels being aligned with an element of the solid-state sensor array, that portion of the radiant energy entering the microchannels parallel to the microchannel walls travels to the sensor element generating an electrical signal from which an image is reconstructed by an external device, and a moving element for movement of the microchannel structure relative to the sample. Discloses a method for scanning samples whereby the sensor array elements trace parallel paths that are arbitrarily close to the parallel paths traced by other elements of the array.

  19. A Computational Framework for High-Throughput Isotopic Natural Abundance Correction of Omics-Level Ultra-High Resolution FT-MS Datasets

    PubMed Central

    Carreer, William J.; Flight, Robert M.; Moseley, Hunter N. B.

    2013-01-01

    New metabolomics applications of ultra-high resolution and accuracy mass spectrometry can provide thousands of detectable isotopologues, with the number of potentially detectable isotopologues increasing exponentially with the number of stable isotopes used in newer isotope tracing methods like stable isotope-resolved metabolomics (SIRM) experiments. This huge increase in usable data requires software capable of correcting the large number of isotopologue peaks resulting from SIRM experiments in a timely manner. We describe the design of a new algorithm and software system capable of handling these high volumes of data, while including quality control methods for maintaining data quality. We validate this new algorithm against a previous single isotope correction algorithm in a two-step cross-validation. Next, we demonstrate the algorithm and correct for the effects of natural abundance for both 13C and 15N isotopes on a set of raw isotopologue intensities of UDP-N-acetyl-D-glucosamine derived from a 13C/15N-tracing experiment. Finally, we demonstrate the algorithm on a full omics-level dataset. PMID:24404440

  20. Multi-constituent determination and fingerprint analysis of Scutellaria indica L. using ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    PubMed

    Liang, Xianrui; Zhao, Cui; Su, Weike

    2015-11-01

    An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry method integrating multi-constituent determination and fingerprint analysis has been established for quality assessment and control of Scutellaria indica L. The optimized method possesses the advantages of speediness, efficiency, and allows multi-constituents determination and fingerprint analysis in one chromatographic run within 11 min. 36 compounds were detected, and 23 of them were unequivocally identified or tentatively assigned. The established fingerprint method was applied to the analysis of ten S. indica samples from different geographic locations. The quality assessment was achieved by using principal component analysis. The proposed method is useful and reliable for the characterization of multi-constituents in a complex chemical system and the overall quality assessment of S. indica. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Trace metals in upland headwater lakes in Ireland.

    PubMed

    Burton, Andrew; Aherne, Julian; Hassan, Nouri

    2013-10-01

    Trace elements (n = 23) in Irish headwater lakes (n = 126) were investigated to determine their ambient concentrations, fractionation (total, dissolved, and non-labile), and geochemical controls. Lakes were generally located in remote upland, acid-sensitive regions along the coastal margins of the country. Total trace metal concentrations were low, within the range of natural pristine surface waters; however, some lakes (~20 %) had inorganic labile aluminum and manganese at levels potentially harmful to aquatic organisms. Redundancy analysis indicated that geochemical weathering was the dominant controlling factor for total metals, compared with acidity for dissolved metals. In addition, many metals were positively correlated with dissolved organic carbon indicating their affinity (or complexation) with humic substances (e.g., aluminum, iron, mercury, lead). However, a number of trace metals (e.g., aluminum, mercury, zinc) were correlated with anthropogenic acidic deposition (i.e., non-marine sulfate), suggesting atmospheric sources or elevated leaching owing to acidic deposition. As transboundary air pollution continues to decline, significant changes in the cycling of trace metals is anticipated.

  2. Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection.

    PubMed

    Xu, Jiao-Jiao; Zhou, Jian; Huang, Bai-Fen; Cai, Zeng-Xuan; Xu, Xiao-Min; Ren, Yi-Ping

    2016-06-01

    A simple and reliable method of ultra high performance liquid chromatography coupled with photo-diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid-phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R(2) ≥ 0.999), acceptable recoveries (80.0-104.4%), and repeatability (RSDs 1.3-10.7%). The limits of detection (21.7-57.4 μg/kg) and quantitation (72.3-191.4 μg/kg) for deoxynivalenols were lower than those usually permitted by various countries' legislation in these food matrices. The method was applied to 34 wheat and rice samples. The results were further compared with results of ultra high performance liquid chromatography with electrospray ionization tandem mass spectrometry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Determination of water traces in various organic solvents using Karl Fischer method under FIA conditions.

    PubMed

    Dantan, N; Frenzel, W; Küppers, S

    2000-05-31

    Flow injection methods utilising the Karl Fischer (KF) reaction with spectrophotometric and potentiometric detection are described for the determination of the trace water content in various organic solvents. Optimisation of the methods resulted in an accessible (linear) working range of 0.01-0.2% water for many solvents studied with a typical precision of 1-2% R.S.D. Only 50 mul of organic solvent was injected and the sampling frequency was about 120 samples per h. Since the slopes of the calibration curves were different for different solvents appropriate calibration was required. Problems associated with spectrophotometric detection and caused by refractive index changes were pointed out and a nested-loop configuration was proposed to overcome this kind of interference. The potentiometric method with a novel flow-through detector cell was shown to surpass the performance of spectrophotometric detection in any respect. The characteristics of the procedures developed made them well applicable for on-line monitoring of technical solvent distillations in an industrial plant.

  4. TraceContract: A Scala DSL for Trace Analysis

    NASA Technical Reports Server (NTRS)

    Barringer, Howard; Havelund, Klaus

    2011-01-01

    In this paper we describe TRACECONTRACT, an API for trace analysis, implemented in the SCALA programming language. We argue that for certain forms of trace analysis the best weapon is a high level programming language augmented with constructs for temporal reasoning. A trace is a sequence of events, which may for example be generated by a running program, instrumented appropriately to generate events. The API supports writing properties in a notation that combines an advanced form of data parameterized state machines with temporal logic. The implementation utilizes SCALA's support for defining internal Domain Specific Languages (DSLs). Furthermore SCALA's combination of object oriented and functional programming features, including partial functions and pattern matching, makes it an ideal host language for such an API.

  5. Determination of trace mercury in water based on N-octylpyridinium ionic liquids preconcentration and stripping voltammetry.

    PubMed

    Li, Zhenhan; Xia, Shanhong; Wang, Jinfen; Bian, Chao; Tong, Jianhua

    2016-01-15

    A novel method for determination of trace mercury in water is developed. The method is performed by extracting mercury firstly with ionic liquids (ILs) and then detecting the concentration of mercury in organic media with anodic stripping voltammetry. Liquid-liquid extraction of mercury(II) ions by four ionic liquids with N-octylpyridinium cations ([OPy](+)) was studied. N-octylpyridinium tetrafluoroborate and N-octylpyridinium trifluoromethylsulfonate were found to be efficient and selective extractant for mercury. Temperature controlled dispersive liquid phase microextraction (TC-DLPME) technique was utilized to improve the performance of preconcentration. After extraction, precipitated IL was diluted by acetonitrile buffer and mercury was detected by differential pulse stripping voltammetry (DPSV) with gold disc electrode. Mercury was enriched by 17 times while interfering ions were reduced by two orders of magnitude in the organic media under optimum condition. Sensitivity and selectivity for electrochemical determination of mercury were improved by using the proposed method. Tap, pond and waste water samples were analyzed with recoveries ranging from 81% to 107% and detection limit of 0.05 μg/L. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Ultra-high-performance liquid chromatography tandem mass spectrometry determination of GHB, GHB-glucuronide in plasma and cerebrospinal fluid of narcoleptic patients under sodium oxybate treatment.

    PubMed

    Tittarelli, Roberta; Pichini, Simona; Pedersen, Daniel S; Pacifici, Roberta; Moresco, Monica; Pizza, Fabio; Busardò, Francesco Paolo; Plazzi, Giuseppe

    2017-05-01

    Sodium oxybate (Xyrem ® ), the sodium salt of γ- hydroxybutyric acid (GHB), is a first-line treatment of the symptoms induced by type 1 narcolepsy (NT1) and it is highly effective in improving sleep architecture, decreasing excessive daytime sleepiness and the frequency of cataplexy attacks. Using an ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) validated method, GHB was determined together with its glucuronide (GHB-gluc), in plasma and cerebrospinal fluid (CSF) samples of NT1 patients under sodium oxybate treatment. To characterize the plasma pharmacokinetics of GHB, three subjects with NT1 were administered at time 0 and 4h with 1.25, 1.5 and 3.55g Xyrem ® , respectively and had their blood samples collected at 7 time points throughout an 8-h session. CSF specimens, collected for orexin A measurement from the same three subjects 6h after their second administration, were also tested. The results obtained suggested that GHB plasma values increased disproportionally with the rising doses, (C max0-4 : 12.53, 32.95 and 69.62μg/mL; C max4-8 : 44.93, 75.03 and 111.93μg/mL for total Xyrem ® dose of 2.5, 3 and 7g respectively) indicating non-linear dose-response. GHB-Gluc was present only in traces in all plasma samples from treated patients, not changing with increasing Xyrem ® doses. GHB values of 5.62, 6.10 and 17.74μg/mL for 2, 3 and 7g Xyrem ® were found in CSF with a significant difference from control values. GHB-Gluc was found in negligible concentrations with no differences to those of control individuals. In conclusion this simple and fast UHPLC-MS/MS method proved useful for pharmacokinetic studies and therapeutic drug monitoring of GHB in narcoleptic patients treated with sodium oxybate. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Quantum Hamiltonian identification from measurement time traces.

    PubMed

    Zhang, Jun; Sarovar, Mohan

    2014-08-22

    Precise identification of parameters governing quantum processes is a critical task for quantum information and communication technologies. In this Letter, we consider a setting where system evolution is determined by a parametrized Hamiltonian, and the task is to estimate these parameters from temporal records of a restricted set of system observables (time traces). Based on the notion of system realization from linear systems theory, we develop a constructive algorithm that provides estimates of the unknown parameters directly from these time traces. We illustrate the algorithm and its robustness to measurement noise by applying it to a one-dimensional spin chain model with variable couplings.

  8. Sensitive determination of trace mercury by UV-visible diffuse reflectance spectroscopy after complexation and membrane filtration-enrichment.

    PubMed

    Yin, Changhai; Iqbal, Jibran; Hu, Huilian; Liu, Bingxiang; Zhang, Lei; Zhu, Bilin; Du, Yiping

    2012-09-30

    A simple, sensitive and selective solid phase reflectometry method is proposed for the determination of trace mercury in aqueous samples. The complexation reagent dithizone was firstly injected into the properly buffered solution with vigorous stirring, which started a simultaneous formation of nanoparticles suspension of dithizone and its complexation reaction with the mercury(II) ions to make Hg-dithizone nanoparticles. After a definite time, the mixture was filtered with membrane, and then quantified directly on the surface of the membrane by using integrating sphere accessory of the UV-visible spectrophotometer. The quantitative analysis was carried out at a wavelength of 485 nm since it yielded the largest difference in diffuse reflectance spectra before and after reaction with mercury(II).A good linear correlation in the range of 0.2-4.0 μg/L with a squared correlation coefficient (R(2)) of 0.9944 and a detection limit of 0.12 μg/L were obtained. The accuracy of the method was evaluated by the analysis of spiked mercury(II) concentrations determined using this method along with those determined by the atomic fluorescence mercury vapourmeter and the results obtained were in good agreement. The proposed method was applied to the determination of mercury in tap water and river water samples with the recovery in an acceptable range (95.7-105.3%). Copyright © 2012 Elsevier B.V. All rights reserved.

  9. [Determination of wilforine in honey using solid phase extraction purification and ultra performance liquid chromatography-tanden mas spectrometry].

    PubMed

    Lei, Meikang; Peng, Fang; Ding, Tao; Zhu, Zitong; Xu, Jiawen; Wu, Xiaoqin

    2015-01-01

    A method based on solid phase extraction and ultra performance liquid chromatography coupled with tandem mass spectrometry (SPE-UPLC-MS/MS) has been proposed for the determination of wilforine residue in honey. After the sample was dissolved with water, concentrated and purified by an HLB solid phase extraction cartridge, the UPLC separation was performed on a Hypersil GOLD C18 column (50 mm x 2.1 mm, 1.9 microm) utilizing a gradient elution program of methanol (containing 0.15% formic acid) and water as mobile phases at a flow rate of 0. 25 mL/min. The determination was carried out with electrospray ion source in the positive mode (ESI) and multiple reaction monitoring (MRM) mode. The mass concentration of wilforine in the range of 0.01-2 microg/L was linearly correlated with the peak area, and the correlation coefficients was greater than 0.998. The limit of quantification (S/N>10) for wilforine was 0.01 microg/kg. The recoveries were 76.1% to 96.2% in the spiked levels of 0.01, 0.05 and 0.5 microg/kg with the relative standard deviations (RSD, n=6) lower than 10%. The results indicate that the method is rapid, sensitive and accurate, and can be applied for the qualitative and quantitative analysis of wilforine in honey.

  10. [Simultaneous determination of 11 bisphenols in plastic bottled drinking water by ultra performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Gou, Xinlei; Gao, Xia; Hu, Guanghui; Chi, Haitao; Le, Shengfeng; Wang, Wei; Liu, Weili

    2014-09-01

    A sensitive method was developed for the simultaneous determination of 11 bisphenols in plastic bottled drinking water by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were freeze-dried under vacuum and then dissolved with methanol. The separation was performed on a UPLC BEH C18 column (100 mm x 2.1 mm, 1.7 μm) by using 0.1% (v/v) NH3 · H2O and methanol as mobile phases with gradient elution at a flow rate of 0.2 mL/min. The electrospray ionization (ESI) source in negative ion mode was used for the analysis of the 11 bisphenols in the multiple reaction monitoring (MRM) mode. The results verified that the standard curves for the 11 bisphenols were obtained with good correlation coefficients (R2) > 0.997 in their concentration ranges. The limits of detection (LOD, S/N = 3) for the 11 bisphenols were in the range of 0.01-1.00 μg/L. The mean recoveries for the 11 bisphenols at three spiked levels (low, middle, high) were 75.3%-102.1% with the relative standard deviations of 1.5%-8.9%. Seven plastic bottled drinking water samples were tested, and no bisphenol was found. The method is accurate, simple, rapid and feasible for the simultaneous determination of bisphenols in plastic bottled drinking water.

  11. Ultra-endurance sports have no negative impact on indices of arterial stiffness.

    PubMed

    Radtke, Thomas; Schmidt-Trucksäss, Arno; Brugger, Nicolas; Schäfer, Daniela; Saner, Hugo; Wilhelm, Matthias

    2014-01-01

    Marathon running has been linked with higher arterial stiffness. Blood pressure is a major contributor to pulse wave velocity (PWV). We examined indices of arterial stiffness with a blood pressure-independent method in marathon runners and ultra-endurance athletes. Male normotensive amateur runners were allocated to three groups according to former participation in competitions: group I (recreational athletes), group II (marathon runners) and group III (ultra-endurance athletes). Indices of arterial stiffness were measured with a non-invasive device (VaSera VS-1500N, Fukuda Denshi, Japan) to determine the cardio-ankle vascular index (CAVI, primary endpoint) and brachial-ankle PWV (baPWV). Lifetime training hours were calculated. Cumulative competitions were expressed as marathon equivalents. Linear regression analysis was performed to determine predictors for CAVI and baPWV. Measurements of arterial stiffness were performed in 51 subjects (mean age 44.6 ± 1.2 years): group I (n = 16), group II (n = 19) and group III (n = 16). No between-group differences existed in age, anthropometric characteristics and resting BP. CAVI and baPWV were comparable between all groups (P = 0.604 and P = 0.947, respectively). In linear regression analysis, age was the only independent predictor for CAVI (R(2) = 0.239, β = 0.455, P = 0.001). Systolic BP was significantly associated with baPWV (R(2) = 0.225, β = 0.403, P = 0.004). In middle-aged normotensive athletes marathon running and ultra-endurance sports had no negative impact on arterial stiffness.

  12. Polymer monolithic capillary microextraction combined on-line with inductively coupled plasma MS for the determination of trace rare earth elements in biological samples.

    PubMed

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

    2013-07-01

    A rapid and sensitive method based on polymer monolithic capillary microextraction combined on-line with microconcentric nebulization inductively coupled plasma MS has been developed for the determination of trace/ultratrace rare earth elements in biological samples. For this purpose, the iminodiacetic acid modified poly(glycidyl methacrylate-trimethylolpropane trimethacrylate) monolithic capillary was prepared and characterized by SEM and FTIR spectroscopy. Factors affecting the extraction efficiency, such as sample pH, sample flow rate, sample/eluent volume, and coexisting ions were investigated in detail. Under the optimal conditions, the LODs for rare earth elements were in the range of 0.08 (Er) to 0.97 ng/L (Nd) with a sampling frequency of 8.5 h(-1), and the RSDs were between 1.5% (Sm) and 7.4% (Nd) (c = 20 ng/L, n = 7). The proposed method was successfully applied to the analysis of trace/ultratrace rare earth elements in human urine and serum samples, and the recoveries for the spiked samples were in the range of 82-105%. The developed method was simple, rapid, sensitive, and favorable for the analysis of trace/ultratrace rare earth elements in biological samples with limited sample volume. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Determination of 82 veterinary drugs in swine waste lagoon sludge by ultra-high performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Li, Xiaowei; Guo, Ping; Shan, Yawen; Ke, Yuebin; Li, Hui; Fu, Qin; Wang, Yingyu; Liu, Tianhe; Xia, Xi

    2017-05-26

    This work reports the development of a multi-residue method for the identification and quantification of 82 veterinary drugs belonging to different chemical classes in swine waste lagoon. The proposed method applies a solid-phase extraction procedure with Oasis PRiME HLB cartridges that combines isolation of the compounds and sample clean-up in a single step. Analysis is performed by ultra-high performance liquid chromatography-tandem mass spectrometry, in one single injection with a chromatographic run time of only 9.5min. Linearity was studied in the range between 1 and 500μgkg -1 using standards prepared both in pure solvent and in the presence of matrix, showing coefficients of determination higher than 0.99 for all the analytes except for cefapirin in matrix. The average recoveries were in the range of 60-110% for most of the compounds tested with inter-day relative standard deviations below 17%. More than 97% of the investigated compounds had less or equal to a 5μgkg -1 quantitation limit in the studied matrix. Finally, the method was used with success to detect and quantify veterinary drugs residues in real samples with sulfonamides, quinolones, and tetracyclines being the most frequently determined compound groups. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Laser ablation ICP-MS profiling and semiquantitative determination of trace element concentrations in desert tortoise shells: documenting the uptake of elemental toxicants.

    PubMed

    Seltzer, Michaeld; Berry, Kristinh

    2005-03-01

    The outer keratin layer (scute) of desert tortoise shells consists of incrementally grown laminae in which various bioaccumulated trace elements are sequestered during scute deposition. Laser ablation ICP-MS examination of laminae in scutes of dead tortoises revealed patterns of trace elemental distribution from which the chronology of elemental uptake can be inferred. These patterns may be of pathologic significance in the case of elemental toxicants such as arsenic, which has been linked to both shell and respiratory diseases. Laser ablation transects, performed along the lateral surfaces of sectioned scutes, offered the most successful means of avoiding exogenous contamination that was present on the scute exterior. Semiquantitative determination of elemental concentrations was achieved using sulfur, a keratin matrix element, as an internal standard. The results presented here highlight the potential of laser ablation ICP-MS as a diagnostic tool for investigating toxic element uptake as it pertains to tortoise morbidity and mortality.

  15. Laser ablation ICP-MS profiling and semiquantitative determination of trace element concentrations in desert tortoise shells: Documenting the uptake of elemental toxicants

    USGS Publications Warehouse

    Seltzer, M.D.; Berry, K.H.

    2005-01-01

    The outer keratin layer (scute) of desert tortoise shells consists of incrementally grown laminae in which various bioaccumulated trace elements are sequestered during scute deposition. Laser ablation ICP-MS examination of laminae in scutes of dead tortoises revealed patterns of trace elemental distribution from which the chronology of elemental uptake can be inferred. These patterns may be of pathologic significance in the case of elemental toxicants such as arsenic, which has been linked to both shell and respiratory diseases. Laser ablation transects, performed along the lateral surfaces of sectioned scutes, offered the most successful means of avoiding exogenous contamination that was present on the scute exterior. Semiquantitative determination of elemental concentrations was achieved using sulfur, a keratin matrix element, as an internal standard. The results presented here highlight the potential of laser ablation ICP-MS as a diagnostic tool for investigating toxic element uptake as it pertains to tortoise morbidity and mortality.

  16. Utility of solid phase spectrophotometry for the modified determination of trace amounts of cadmium in food samples.

    PubMed

    Amin, Alaa S; Gouda, Ayman A

    2012-05-01

    A modified selective, highly sensitive and accurate procedure for the determination of trace amounts of cadmium which reacts with 1-(2-benzothiazolylazo)-2-hydroxy-3-naphthoic acid (BTAHNA) to give a deep violet complex with high molar absorptivity (7.05×10(6)Lmol(-1) cm(-1), 3.92×10(7)Lmol(-1)cm(-1), 1.78×10(8)Lmol(-1)cm(-1), and 4.10×10(8)Lmol(-1)cm(-1)), fixed on a Dowex 1-X8 type anion-exchange resin for 10mL, 100mL, 500mL, and 1000mL, respectively. Calibration is linear over the range 0.2-3.5μgL(-1) with RSD of ⩽1.14% (n=10). The detection and quantification limits were calculated. Increasing the sample volume can enhance the sensitivity. The method has been successfully applied for the determination of Cd(II) in food samples, water samples and some salts samples without interfering effect of various cations and anions. Copyright © 2011 Elsevier Ltd. All rights reserved.

  17. Development, validation and application of an ICP-MS/MS method to quantify minerals and (ultra-)trace elements in human serum.

    PubMed

    Meyer, Sören; Markova, Mariya; Pohl, Gabriele; Marschall, Talke A; Pivovarova, Olga; Pfeiffer, Andreas F H; Schwerdtle, Tanja

    2018-09-01

    Multi-element determination in human samples is very challenging. Especially in human intervention studies sample volumes are often limited to a few microliters and due to the high number of samples a high-throughput is indispensable. Here, we present a state-of-the-art ICP-MS/MS-based method for the analysis of essential (trace) elements, namely Mg, Ca, Fe, Cu, Zn, Mo, Se and I, as well as food-relevant toxic elements such as As and Cd. The developed method was validated regarding linearity of the calibration curves, method LODs and LOQs, selectivity and trueness as well as precision. The established reliable method was applied to quantify the element serum concentrations of participants of a human intervention study (LeguAN). The participants received isocaloric diets, either rich in plant protein or in animal protein. While the serum concentrations of Mg and Mo increased in participants receiving the plant protein-based diet (above all legumes), the Se concentration in serum decreased. In contrast, the animal protein-based diet, rich in meat and dairy products, resulted in an increased Se concentration in serum. Copyright © 2018 Elsevier GmbH. All rights reserved.

  18. Rapid Determination of Bile Acids in Bile from Various Mammals by Reversed-Phase Ultra-Fast Liquid Chromatography.

    PubMed

    Si, Gu Leng Ri; Yao, Peng; Shi, Luwen

    2015-08-01

    A valid and efficient reversed-phase ultra-fast liquid chromatography method was developed for the simultaneous determination of 13 bile acids in the bile of three mammal species, including rat, pig and human gallstone patients. Chromatographic separation was performed with a Shim-pack XR-ODS column, and the mobile phase consisted of acetonitrile and potassium phosphate buffer (pH 2.6) at a flow rate of 0.5 mL min(-1). The linear detection range of most bile acids ranged from 2 to 600 ng µL(-1) with a good correlation coefficient (>0.9995). The precision of each bile acid was <1.8% for intraday and <4.8% for interday. All bile acids were separated in 15 min with satisfactory resolution, and the total analysis time was 18 min, including equilibration. The method was successfully applied in rapid screening of bile samples from the three mammals. Significant metabolic frameworks of bile acids among various species were observed, whereas considerable quantitative variations in both inter- and intraspecies were also observed, especially for gallstone patients. Our results suggest that detecting the change of bile acid profiles could be applied for the diagnosis of gallstone disease. © Crown copyright 2014.

  19. Ultra-reducing conditions in average mantle peridotites and in podiform chromitites: a thermodynamic model for moissanite (SiC) formation

    NASA Astrophysics Data System (ADS)

    Golubkova, Anastasia; Schmidt, Max W.; Connolly, James A. D.

    2016-05-01

    and the limited diffusive equilibration of SiC with most minerals in the rocks indicate temperatures below 700-800 °C. Moissanite from mantle environments is hence a mineral that does not inform on pressure but on a low to moderate temperature environment involving ultra-reduced fluids. Any mineral in equilibrium with SiC could only contain traces of Fe2+ or Cr3+.

  20. Future ultra-speed tube-flight

    NASA Astrophysics Data System (ADS)

    Salter, Robert M.

    1994-05-01

    Future long-link, ultra-speed, surface transport systems will require electromagnetically (EM) driven and restrained vehicles operating under reduced-atmosphere in very straight tubes. Such tube-flight trains will be safe, energy conservative, pollution-free, and in a protected environment. Hypersonic (and even hyperballistic) speeds are theoretically achievable. Ultimate system choices will represent tradeoffs between amoritized capital costs (ACC) and operating costs. For example, long coasting links might employ aerodynamic lift coupled with EM restraint and drag make-up. Optimized, combined EM lift, and thrust vectors could reduce energy costs but at increased ACC. (Repulsive levitation can produce lift-over-drag l/d ratios a decade greater than aerodynamic), Alternatively, vehicle-emanated, induced-mirror fields in a conducting (aluminum sheet) road bed could reduce ACC but at substantial energy costs. Ultra-speed tube flight will demand fast-acting, high-precision sensors and computerized magnetic shimming. This same control system can maintain a magnetic 'guide way' invariant in inertial space with inertial detectors imbedded in tube structures to sense and correct for earth tremors. Ultra-speed tube flight can complete with aircraft for transit time and can provide even greater passenger convenience by single-model connections with local subways and feeder lines. Although cargo transport generally will not need to be performed at ultra speeds, such speeds may well be desirable for high throughput to optimize channel costs. Thus, a large and expensive pipeline might be replaced with small EM-driven pallets at high speeds.

  1. Future ultra-speed tube-flight

    NASA Technical Reports Server (NTRS)

    Salter, Robert M.

    1994-01-01

    Future long-link, ultra-speed, surface transport systems will require electromagnetically (EM) driven and restrained vehicles operating under reduced-atmosphere in very straight tubes. Such tube-flight trains will be safe, energy conservative, pollution-free, and in a protected environment. Hypersonic (and even hyperballistic) speeds are theoretically achievable. Ultimate system choices will represent tradeoffs between amoritized capital costs (ACC) and operating costs. For example, long coasting links might employ aerodynamic lift coupled with EM restraint and drag make-up. Optimized, combined EM lift, and thrust vectors could reduce energy costs but at increased ACC. (Repulsive levitation can produce lift-over-drag l/d ratios a decade greater than aerodynamic), Alternatively, vehicle-emanated, induced-mirror fields in a conducting (aluminum sheet) road bed could reduce ACC but at substantial energy costs. Ultra-speed tube flight will demand fast-acting, high-precision sensors and computerized magnetic shimming. This same control system can maintain a magnetic 'guide way' invariant in inertial space with inertial detectors imbedded in tube structures to sense and correct for earth tremors. Ultra-speed tube flight can complete with aircraft for transit time and can provide even greater passenger convenience by single-model connections with local subways and feeder lines. Although cargo transport generally will not need to be performed at ultra speeds, such speeds may well be desirable for high throughput to optimize channel costs. Thus, a large and expensive pipeline might be replaced with small EM-driven pallets at high speeds.

  2. The Levels of Trace Elements in Honey and Molasses Samples That Were Determined by ICP-OES After Microwave Digestion Method.

    PubMed

    Altundag, Huseyin; Bina, Emel; Altıntıg, Esra

    2016-04-01

    The aim of this study is determining the amount of Al, Cu, Fe, Mn, Ni, Pb and Zn in samples of molasses and honey which were gathered from the Sakarya and Istanbul regions. In this study, trace elements in 8 honey and 20 molasses samples with different botanic features were evaluated. The sample preparation phase was performed via wet decomposition method and microwave digestion system. The accuracy of the method was checked by the standard reference material; tea leaves (INCY-TL-1) and NIST-SRM 1515-apple. The concentrations of essential trace elements (TEs) were observed in the range of 1.61 ± 0.01-287.03 ± 1.07; 0.21 ± 0.01-11.04 ± 0.12; 0.35 ± 0.03-21.71 ± 0.02 and 1.19 ± 0.01-60.90 ± 1.09 μg g(-1) for iron, copper, manganese and zinc ions, respectively, while the toxic element contents were observed in the range of 0.82 ± 0.17-3.06 ± 0.03; 0.04 ± 0.05-1.96 ± 0.03 and 0.62 ± 0.01-120.52 ± 0.10 μg g(-1) for lead, nickel and aluminum ions, respectively. The concentrations of basic TEs iron, copper, manganese and zinc were determined as 3.87 ± 0.04-16.76 ± 0.06; 0.45 ± 0.03-2.15 ± 0.01; 0.13 ± 0.01-15.02 ± 0.14 and 0.80 ± 0.09-12.03 ± 0.19 for honey samples. Also, toxic metal, lead, nickel and aluminum values in the honey samples were determined as 1.21 ± 0.12-2.46 ± 0.21; 0.28 ± 0.14-0.88 ± 0.43 and 2.11 ± 0.02-8.04 ± 0.08. A comparison between gathered data and literature values has performed and it is determined that such findings are suitable with the literature.

  3. [Direct determination of ethyl carbamate in Chinese rice wine and grape wine by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry].

    PubMed

    Wang, Lijuan; Ke, Runhui; Wang, Bing; Yin, Jianjun; Song, Quanhou

    2012-09-01

    An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometric (UPLC-ESI-MS/MS) method was established for the direct determination of ethyl carbamate in Chinese rice wine and grape wine. The Chinese rice wine and grape wine samples were diluted with distilled water, filtered through 0. 22 microm microporous membrane. The LC separation was performed on a Waters Acquity UPLC system with a BEH C18 column, acetonitrile and 0. 1% (v/v) acetic acid aqueous solution as the mobile phase. The ethyl carbamate was determined in the mode of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). The butyl carbamate (BC) was used as the internal standard for the quantitative determination. The calibration curve showed good linearity in the range of 2 - 500 microg/L with the correlation coefficient greater than 0.995. The limit of detection (LOD) was 1.7 microg/L and the limit of quantification (LOQ) was 5.0 microg/L. The recoveries of the ethyl carbamate in Chinese rice wine and grape wine was in the range of 90% - 102%. The relative standard deviations (RSDs) of intra-day and inter-day determinations were 0. 8% - 4.5% and 1.4% - 5.6% (n = 6). The results indicated that the proposed method is easy, fast, sensitive, and suitable for the determination of ethyl carbamate in Chinese rice wine and grape wine.

  4. CO2 and vitamin B12 interactions determine bioactive trace metal requirements of a subarctic Pacific diatom.

    PubMed

    King, Andrew L; Sañudo-Wilhelmy, Sergio A; Leblanc, Karine; Hutchins, David A; Fu, Feixue

    2011-08-01

    Phytoplankton growth can be limited by numerous inorganic nutrients and organic growth factors. Using the subarctic diatom Attheya sp. in culture studies, we examined how the availability of vitamin B(12) and carbon dioxide partial pressure (pCO(2)) influences growth rate, primary productivity, cellular iron (Fe), cobalt (Co), zinc (Zn) and cadmium (Cd) quotas, and the net use efficiencies (NUEs) of these bioactive trace metals (mol C fixed per mol cellular trace metal per day). Under B(12)-replete conditions, cells grown at high pCO(2) had lower Fe, Zn and Cd quotas, and used those trace metals more efficiently in comparison with cells grown at low pCO(2). At high pCO(2), B(12)-limited cells had ~50% lower specific growth and carbon fixation rates, and used Fe ~15-fold less efficiently, and Zn and Cd ~3-fold less efficiently, in comparison with B(12)-replete cells. The observed higher Fe, Zn and Cd NUE under high pCO(2)/B(12)-replete conditions are consistent with predicted downregulation of carbon-concentrating mechanisms. Co quotas of B(12)-replete cells were ∼5- to 14-fold higher in comparison with B(12)-limited cells, suggesting that >80% of cellular Co of B(12)-limited cells was likely from B(12). Our results demonstrate that CO(2) and vitamin B(12) interactively influence growth, carbon fixation, trace metal requirements and trace metal NUE of this diatom. This suggests the need to consider complex feedback interactions between multiple environmental factors for this biogeochemically critical group of phytoplankton in the last glacial maximum as well as the current and future changing ocean.

  5. Trace element release from estuarine sediments of South Mosquito Lagoon near Kennedy Space Center

    NASA Technical Reports Server (NTRS)

    Menon, M. P.; Ghuman, G. S.; Emeh, C. O.

    1979-01-01

    Analytical partitioning of four trace metals in estuarine sediments collected from eight sites in South Mosquito Lagoon near Kennedy Space Center, in terms of four different categories was accomplished using four different extraction techniques. The concentrations of the four trace metals, Zn, Mn, Cd, and Cu, released in interstitial water extract, 1 N ammonium acetate extract, conc. HCl extract and fusion extract of sediments as well as their concentrations in water samples collected from the same location were determined using flame atomic absorption technique. From the analytical results the percentages of total amount of each metal distributed among four different categories, interstitial water phase, acetate extractable, acid extractable and detrital crystalline material, were determined. Our results suggest that analytical partitioning of trace metals in estuarine sediments may be used to study the mechanism of incorporation of trace metals with sediments from natural waters. A correlation between the seasonal variation in the concentration of acetate extractable trace metals in the sediment and similar variation in their concentration in water was observed. A mechanism for the release of trace metals from estuarine sediments to natural water is also suggested.

  6. Pathfinder Photogrammetry Research for Ultra-Lightweight and Inflatable Space Structures

    NASA Technical Reports Server (NTRS)

    Giersch, Louis Roy Miller

    2001-01-01

    The defining characteristic of ultra-lightweight and inflatable space structures is that they are both very large and very low mass. This makes standard contacting methods of measurement (e.g. attaching accelerometers) impractical because the dynamics of the structure would be changed by the mass of the contacting instrument. Optical measurements are therefore more appropriate. Photogrammetry is a leading candidate for the optical analysis of gossamer structures because it allows for the measurement of a large number of points, is amenable to time sequences, and offers the potential for a high degree of accuracy. The purpose of this thesis is to develop the methodology and determine the effectiveness of a photogrammetry system in measuring ultra-lightweight and inflatable space structures. The results of this thesis will be considered in the design of an automated photogrammetry system for the l6m-diameter vacuum chamber at the NASA Langley Research Center.

  7. Electrochemical Corrosion Properties of Commercial Ultra-Thin Copper Foils

    NASA Astrophysics Data System (ADS)

    Yen, Ming-Hsuan; Liu, Jen-Hsiang; Song, Jenn-Ming; Lin, Shih-Ching

    2017-08-01

    Ultra-thin electrodeposited Cu foils have been developed for substrate thinning for mobile devices. Considering the corrosion by residual etchants from the lithography process for high-density circuit wiring, this study investigates the microstructural features of ultra-thin electrodeposited Cu foils with a thickness of 3 μm and their electrochemical corrosion performance in CuCl2-based etching solution. X-ray diffraction and electron backscatter diffraction analyses verify that ultra-thin Cu foils exhibit a random texture and equi-axed grains. Polarization curves show that ultra-thin foils exhibit a higher corrosion potential and a lower corrosion current density compared with conventional (220)-oriented foils with fan-like distributed fine-elongated columnar grains. Chronoamperometric results also suggest that ultra-thin foils possess superior corrosion resistance. The passive layer, mainly composed of CuCl and Cu2O, forms and dissolves in sequence during polarization.

  8. Ultra-weak sector, Higgs boson mass, and the dilaton

    DOE PAGES

    Allison, Kyle; Hill, Christopher T.; Ross, Graham G.

    2014-09-26

    The Higgs boson mass may arise from a portal coupling to a singlet fieldmore » $$\\sigma$$ which has a very large VEV $$f \\gg m_\\text{Higgs}$$. This requires a sector of "ultra-weak" couplings $$\\zeta_i$$, where $$\\zeta_i \\lesssim m_\\text{Higgs}^2 / f^2$$. Ultra-weak couplings are technically naturally small due to a custodial shift symmetry of $$\\sigma$$ in the $$\\zeta_i \\rightarrow 0$$ limit. The singlet field $$\\sigma$$ has properties similar to a pseudo-dilaton. We engineer explicit breaking of scale invariance in the ultra-weak sector via a Coleman-Weinberg potential, which requires hierarchies amongst the ultra-weak couplings.« less

  9. Effects of psilocybin on hippocampal neurogenesis and extinction of trace fear conditioning.

    PubMed

    Catlow, Briony J; Song, Shijie; Paredes, Daniel A; Kirstein, Cheryl L; Sanchez-Ramos, Juan

    2013-08-01

    Drugs that modulate serotonin (5-HT) synaptic concentrations impact neurogenesis and hippocampal (HPC)-dependent learning. The primary objective is to determine the extent to which psilocybin (PSOP) modulates neurogenesis and thereby affects acquisition and extinction of HPC-dependent trace fear conditioning. PSOP, the 5-HT2A agonist 25I-NBMeO and the 5-HT2A/C antagonist ketanserin were administered via an acute intraperitoneal injection to mice. Trace fear conditioning was measured as the amount of time spent immobile in the presence of the conditioned stimulus (CS, auditory tone), trace (silent interval) and post-trace interval over 10 trials. Extinction was determined by the number of trials required to resume mobility during CS, trace and post-trace when the shock was not delivered. Neurogenesis was determined by unbiased counts of cells in the dentate gyrus of the HPC birth-dated with BrdU co-expressing a neuronal marker. Mice treated with a range of doses of PSOP acquired a robust conditioned fear response. Mice injected with low doses of PSOP extinguished cued fear conditioning significantly more rapidly than high-dose PSOP or saline-treated mice. Injection of PSOP, 25I-NBMeO or ketanserin resulted in significant dose-dependent decreases in number of newborn neurons in hippocampus. At the low doses of PSOP that enhanced extinction, neurogenesis was not decreased, but rather tended toward an increase. Extinction of "fear conditioning" may be mediated by actions of the drugs at sites other than hippocampus such as the amygdala, which is known to mediate the perception of fear. Another caveat is that PSOP is not purely selective for 5-HT2A receptors. PSOP facilitates extinction of the classically conditioned fear response, and this, and similar agents, should be explored as potential treatments for post-traumatic stress disorder and related conditions.

  10. Trace elements in sera of patients with hepatitis B: Determination and analysis

    NASA Astrophysics Data System (ADS)

    Saod, Wahran M.; Darwish, Nadiya T.; Zaidan, Tahseen A.; Alfalujie, Abdul Wahab A.

    2018-04-01

    Chronic Hepatitis B (HBV) is the leading cause of morbidity and mortality worldwide with about 248 million people having HBV infection. Trace elements e.g. copper (Cu), zinc (Zn), selenium (Se) and iron (Fe) are constituent components of many metal proteins and metalloenzymes in human sera. Therefore, the ratios of these trace elements in human sera are often stated to be a good marker for diagnosing various diseases including HBV. The aims of this study are: to compare the level of trace elements in sera of patients infected with HBV and healthy participants, and to evaluate the efficiency of analytical techniques (e.g. Inductively Coupled Plasma-Mass spectrometry (ICP-MS), Atomic Absorption Spectroscopy (hydride generation) (AAS) and Graphite Furnace Atomic Absorption Spectroscopy (GFAAS) that are currently used to detect Fe and Se elements in Patients' human sera. The findings of this study show that the concentration range of copper element between (132.80±28.64 µg/dl) to (105.66±23.20 µg/dl) was significantly higher in HBV infected patients as compared to those in healthy controls (91.27±9.20 µg/dl). Iron concentration range between (206.64±61.60 µg/l) to (170.00±36.71 µg/l) was significantly higher in HBV infected patients as compared to those in healthy controls (158.00±15.13 µg/l). However, patients with HBV had significantly lower serum concentrations of zinc with a concentration range between (111.64±20.90 µg/dl) to (99.25±24.06 µg/dl) as compared to those in healthy controls (113.44±16.38 µg/dl). While selenium concentration range between (64.39±7.39 µg/l) to (51.10±4.96 µg/l) was significantly lower in HBV infected patients as compared to those in healthy controls (67.68±7.60) (μg/l). Moreover, the results of this study suggest that (AAS) technique was the most accurate method to measure the concentration of selenium element, while (UV and ICP-MS) analytical techniques have the same efficiency in measuring the iron concentration.

  11. Traces of ternary relations

    NASA Astrophysics Data System (ADS)

    Zedam, Lemnaouar; Barkat, Omar; De Baets, Bernard

    2018-05-01

    In this paper, we generalize the notion of traces of a binary relation to the setting of ternary relations. With a given ternary relation, we associate three binary relations: its left, middle and right trace. As in the binary case, these traces facilitate the study and characterization of properties of a ternary relation. Interestingly, the traces themselves turn out to be the greatest solutions of relational inequalities associated with newly introduced compositions of a ternary relation with a binary relation (and vice versa).

  12. Polymer monolithic capillary microextraction on-line coupled with inductively coupled plasma-mass spectrometry for the determination of trace Au and Pd in biological samples

    NASA Astrophysics Data System (ADS)

    Liu, Xiaolan; He, Man; Chen, Beibei; Hu, Bin

    2014-11-01

    A novel method based on on-line polymer monolithic capillary microextraction (CME)-inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Au and Pd in biological samples. For this purpose, poly(glycidyl methacrylate-ethylene dimethacrylate) monolith was prepared and functionalized with mercapto groups. The prepared monolith exhibited good selectivity to Au and Pd, and good resistance to strong acid with a long life span. Factors affecting the extraction efficiency of CME, such as sample acidity, sample flow rate, eluent conditions and coexisting ion interference were investigated in detail. Under the optimal conditions, the limits of detection (LODs, 3σ) were 5.9 ng L- 1 for Au and 8.3 ng L- 1 for Pd, and the relative standard deviations (RSDs, c = 50 ng L-1, n = 7) were 6.5% for Au and 1.1% for Pd, respectively. The developed method was successfully applied to the determination of Au and Pd in human urine and serum samples with the recovery in the range of 84-118% for spiked samples. The developed on-line polymer monolithic CME-ICP-MS method has the advantages of rapidity, simplicity, low sample/reagent consumption, high sensitivity and is suitable for the determination of trace Au and Pd in biological samples with limited amount available and complex matrix.

  13. Determination of atmospheric organosulfates using HILIC chromatography with MS detection

    NASA Astrophysics Data System (ADS)

    Hettiyadura, A. P. S.; Stone, E. A.; Kundu, S.; Baker, Z.; Geddes, E.; Richards, K.; Humphry, T.

    2015-06-01

    Measurements of organosulfates in ambient aerosols provide insight to the extent of secondary organic aerosol (SOA) formation from mixtures of biogenic gases and anthropogenic pollutants. Organosulfates have, however, proved analytically challenging to quantify, due to lack of authentic standards and the complex sample matrix in which organosulfates are observed. This study presents a sensitive and accurate new analytical method for the quantification of organosulfates based upon ultra-performance liquid chromatography (UPLC) with negative electrospray ionization mass spectrometry (MS) with the aid of synthesized organosulfate standards. The separation is based upon hydrophilic interaction liquid chromatography (HILIC) with an amide stationary phase that provides excellent retention of carboxy-organosulfates and isoprene-derived organosulfates. The method is validated using six model compounds: methyl sulfate, ethyl sulfate, benzyl sulfate, hydroxyacetone sulfate, lactic acid sulfate and glycolic acid sulfate. A straightforward protocol for synthesis of highly pure organosulfate potassium salts for use as quantification standards is presented. This method is used to evaluate the efficiency and precision of two methods of ambient PM2.5 sample extraction. Spike recoveries averaged 98 ± 8% for extraction by ultra-sonication and 98 ± 10% for extraction by rotary shaking. Ultra-sonication was determined to be a better method due to its higher precision compared to rotary shaking. Analysis of ambient PM2.5 samples collected on 10-11 July 2013 in Centreville, AL, USA during the Southeast Atmosphere Study (SAS) confirms the presence of hydroxyacetone sulfate in ambient aerosol for the first time. Lactic acid sulfate was the most abundant compound measured (9.6-19 ng m-3), followed by glycolic acid sulfate (8-14 ng m-3) and hydroxyacetone sulfate (2.7-5.8 ng m-3). Trace amounts of methyl sulfate were detected, while ethyl sulfate and benzyl sulfate were not. Application

  14. Rapid determination of the various native forms of vitamin B6 and B2 in cow's milk using ultra-high performance liquid chromatography.

    PubMed

    Schmidt, A; Schreiner, M G; Mayer, H K

    2017-06-02

    As the formation of pyridoxal phosphate, the active cofactor of vitamin B 6 , is dependent on riboflavin 5-phosphate, we propose a fast and simple ultra-high performance liquid chromatography method for the simultaneous determination of the native B 6 vitamers pyridoxal, pyridoxine, pyridoxamine, their mono phosphorus esters and 4-pyridoxic acid as well as vitamin B 2 as riboflavin and its phosphorus ester riboflavin 5-phosphate in milk. Separation was achieved under 6.0min by reversed-phase and pH gradient elution. Sample preparation was optimized regarding various acids and pH levels. Changes in those parameters led to significant deviations of sample matrix breakdown efficiency. The optimized method was then validated regarding specificity, accuracy, precision, linearity, range, detection and quantification limits. As the method performed satisfactory, is was used to study commercial liquid cow's milk (n=31), regarding effects of the employed preservation technique (pasteurization, extended shelf-life, ultra-high temperature) on the composition and content of B 6 and B 2 vitamers. In cow's milk, vitamin B 6 mostly consists of pyridoxal and its phosphate ester, with pyridoxal phosphate being the bulk component. The catabolite of the vitamin B 6 metabolism, 4-pyridoxic acid was present in significant amounts in all studied samples, with up to 2.69μmolL -1 . Vitamin B 2 was present as riboflavin and its phosphate ester up to 12.86μmolL -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

  15. A primer on trace metal-sediment chemistry

    USGS Publications Warehouse

    Horowitz, Arthur J.

    1985-01-01

    In most aquatic systems, concentrations of trace metals in suspended sediment and the top few centimeters of bottom sediment are far greater than concentrations of trace metals dissolved in the water column. Consequently, the distribution, transport, and availability of these constituents can not be intelligently evaluated, nor can their environmental impact be determined or predicted solely through the sampling and analysis of dissolved phases. This Primer is designed to acquaint the reader with the basic principles that govern the concentration and distribution of trace metals associated with bottom and suspended sediments. The sampling and analysis of suspended and bottom sediments are very important for monitoring studies, not only because trace metal concentrations associated with them are orders of magnitude higher than in the dissolved phase, but also because of several other factors. Riverine transport of trace metals is dominated by sediment. In addition, bottom sediments serve as a source for suspended sediment and can provide a historical record of chemical conditions. This record will help establish area baseline metal levels against which existing conditions can be compared. Many physical and chemical factors affect a sediment's capacity to collect and concentrate trace metals. The physical factors include grain size, surface area, surface charge, cation exchange capacity, composition, and so forth. Increases in metal concentrations are strongly correlated with decreasing grain size and increasing surface area, surface charge, cation exchange capacity, and increasing concentrations of iron and manganese oxides, organic matter, and clay minerals. Chemical factors are equally important, especially for differentiating between samples having similar bulk chemistries and for inferring or predicting environmental availability. Chemical factors entail phase associations (with such sedimentary components as interstitial water, sulfides, carbonates, and organic

  16. Traces of Drosophila Memory

    PubMed Central

    Davis, Ronald L.

    2012-01-01

    Summary Studies using functional cellullar imaging of living flies have identified six memory traces that form in the olfactory nervous system after conditioning with odors. These traces occur in distinct nodes of the olfactory nervous system, form and disappear across different windows of time, and are detected in the imaged neurons as increased calcium influx or synaptic release in response to the conditioned odor. Three traces form at, or near acquisition and co-exist with short-term behavioral memory. One trace forms with a delay after learning and co-exists with intermediate-term behavioral memory. Two traces form many hours after acquisition and co-exist with long-term behavioral memory. The transient memory traces may support behavior across the time-windows of their existence. The experimental approaches for dissecting memory formation in the fly, ranging from the molecular to the systems, make it an ideal system for dissecting the logic by which the nervous system organizes and stores different temporal forms of memory. PMID:21482352

  17. Ultra-High Performance Liquid Chromatography (UHPLC) Method for the Determination of Limonene in Sweet Orange (Citrus sinensis) Oil: Implications for Limonene Stability.

    PubMed

    Bernart, Matthew W

    2015-01-01

    The citrus-derived bioactive monoterpene limonene is an important industrial commodity and fragrance constituent. An RP isocratic elution C18 ultra-HPLC (UHPLC) method using a superficially porous stationary phase and photodiode array (PDA) detector has been developed for determining the limonene content of sweet orange (Citrus sinensis) oil. The method is fast with a cycle time of 1.2 min, linear, precise, accurate, specific, and stability indicating, and it satisfies U.S. Pharmacopeia suitability parameters. The method may be useful in its present form for limonene processing, or modified for research on more polar compounds of the terpenome. A forced-degradation experiment showed that limonene is degraded by heat in hydro-ethanolic solution. PDA detection facilitates classification of minor components of the essential oil, including β-myrcene.

  18. Atmospheric Deposition of Trace Elements in Ombrotrophic Peat as a Result of Anthropic Activities

    NASA Astrophysics Data System (ADS)

    Fabio Lourençato, Lucio; Cabral Teixeira, Daniel; Vieira Silva-Filho, Emmanoel

    2014-05-01

    is determined by calcination and pH. For the determination of mercury, an aliquot of 10 mL of sample with 5 mL of the reducing agent 2 % SnCl2, purged with air by atomic absorption spectrophotometry by cold vapor, EAAVF is being used. The determination of other trace elements (Zn, Cd and Pb) is analyzed by flame atomic absorption spectroscopy (FAAS).

  19. [Simultaneous determination of 22 typical pharmaceuticals and personal care products in environmental water using ultra performance liquid chromatography- triple quadrupole mass spectrometry].

    PubMed

    Wu, Chunying; Gu, Feng; Bai, Lu; Lu, Wenlong

    2015-08-01

    An analytical method for simultaneous determination of 22 typical pharmaceuticals and personal care products (PPCPs) in environmental water samples was developed by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). An Oasis HLB solid phase extraction cartridge, methanol as washing solution, water containing 0. 1% formic acid-methanol (7:3, v/v) as the mobile phases were selected for sample pretreatment and chromatographic separation. Based on the optimized sample pretreatment procedures and separation condition, the target recoveries ranged from 73% to 125% in water with the relative standard deviations ( RSDs) from 8.8% to 17.5%, and the linear ranges were from 2 to 2 000 µg/L with correlation coefficients (R2) not less than 0.997. The method can be applied to simultaneous determination of the 22 typical PPCPs in environmental water samples because of its low detection limits and high recoveries. It can provide support and help for the related research on water environmental risk assessment and control of the micro-organic pollutants.

  20. Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

    NASA Astrophysics Data System (ADS)

    Batanova, V. G.; Sobolev, A. V.; Magnin, V.

    2018-01-01

    Use of the electron probe microanalyser (EPMA) for trace element analysis has increased over the last decade, mainly because of improved stability of spectrometers and the electron column when operated at high probe current; development of new large-area crystal monochromators and ultra-high count rate spectrometers; full integration of energy-dispersive / wavelength-dispersive X-ray spectrometry (EDS/WDS) signals; and the development of powerful software packages. For phases that are stable under a dense electron beam, the detection limit and precision can be decreased to the ppm level by using high acceleration voltage and beam current combined with long counting time. Data on 10 elements (Na, Al, P, Ca, Ti, Cr, Mn, Co, Ni, Zn) in olivine obtained on a JEOL JXA-8230 microprobe with tungsten filament show that the detection limit decreases proportionally to the square root of counting time and probe current. For all elements equal or heavier than phosphorus (Z = 15), the detection limit decreases with increasing accelerating voltage. The analytical precision for minor and trace elements analysed in olivine at 25 kV accelerating voltage and 900 nA beam current is 4 - 18 ppm (2 standard deviations of repeated measurements of the olivine reference sample) and is similar to the detection limit of corresponding elements. To analyse trace elements accurately requires careful estimation of background, and consideration of sample damage under the beam and secondary fluorescence from phase boundaries. The development and use of matrix reference samples with well-characterised trace elements of interest is important for monitoring and improving of the accuracy. An evaluation of the accuracy of trace element analyses in olivine has been made by comparing EPMA data for new reference samples with data obtained by different in-situ and bulk analytical methods in six different laboratories worldwide. For all elements, the measured concentrations in the olivine reference sample

  1. Soluble trace elements and total mercury in Arctic Alaskan snow

    USGS Publications Warehouse

    Snyder-Conn, E.; Garbarino, J.R.; Hoffman, G.L.; Oelkers, A.

    1997-01-01

    Ultraclean field and laboratory procedures were used to examine trace element concentrations in northern Alaskan snow. Sixteen soluble trace elements and total mercury were determined in snow core samples representing the annual snowfall deposited during the 1993-94 season at two sites in the Prudhoe Bay oil field and nine sites in the Arctic National Wildlife Refuge (Arctic NWR). Results indicate there were two distinct point sources for trace elements in the Prudhoe Bay oil field - a source associated with oil and gas production and a source associated with municipal solid-waste incineration. Soluble trace element concentrations measured in snow from the Arctic NWR resembled concentrations of trace elements measured elsewhere in the Arctic using clean sample-collection and processing techniques and were consistent with deposition resulting from widespread arctic atmospheric contamination. With the exception of elements associated with sea salts, there were no orographic or east-west trends observed in the Arctic NWR data, nor were there any detectable influences from the Prudhoe Bay oil field, probably because of the predominant easterly and northeasterly winds on the North Slope of Alaska. However, regression analysis on latitude suggested significant south-to-north increases in selected trace element concentrations, many of which appear unrelated to the sea salt contribution.

  2. Tracing Evolution of Starbursts and AGNs using Ultra-deep Radio and mm/smm Surveys

    NASA Astrophysics Data System (ADS)

    Yun, Min S.; Gim, Hansung; Morrison, Glenn; Hales, Christopher A.; Momjian, Emmanuel; Owen, Frazer; Kellermann, Ken; Aretxaga, Itziar; Giavalisco, Mauro; Hughes, David; Lowenthal, James; Miller, Neal; Kawabe, Ryohei; Kohno, Kotaro

    2015-08-01

    There is growing evidence supporting a rapid build up of metals among massive galaxies during their rapid growth via an intense starburst in the early epochs. These star formation activities may be largely obscured in the UV and optical light, as in the local universe. If the growth of supermassive blackholes occurs at or nearly the same time, the accompanying AGN activity may also be heavily obscured. Ultra-deep surveys in the radio and far-infrared can offer extinction-free view of these systems, and the advent of new facilities such as the Jansky VLA, ALMA, and LMT now allows us to probe directly the population of starburst galaxies that are responsible for the bulk of the stellar mass build-up during the epoch of galaxy growth (SFR > 10-100 M⊙/yr at z≈2 or earlier). We will present our analysis of the properties of the micro-Jansky radio sources identified by new Jansky VLA surveys of the GOODS and COSMOS fields using the rich archival data already available (Herschel, Spitzer, Chandra, ALMA, LMT, etc.). Specifically, we find evidence for two populations of microJy radio sources with distinct spectral index distribution. We explore whether this reflects differences in the underlying powering mechanisms by examining their radio-FIR correlation and X-ray properties. We also find the previously reported apparent systematic change in the "q-value" with increasing redshift, and we examine the reality of this trend in some detail. Finally, we will also examine the spatial extent of activities for a subset of the sample where high angular resolution (better than 1") information is available.

  3. The simple determination method for anthocyanidin aglycones in fruits using ultra-high-performance liquid chromatography.

    PubMed

    Shim, You-Shin; Yoon, Won-Jin; Kim, Dong-Man; Watanabe, Masaki; Park, Hyun-Jin; Jang, Hae Won; Lee, Jangho; Ha, Jaeho

    2015-01-01

    The simple determination method for anthocyanidin aglycones in fruits using ultra-high-performance liquid chromatography (UHPLC) coupled with the heating-block acidic hydrolysis method was validated through the precision, accuracy and linearity. The UHPLC separation was performed on a reversed-phase C18 column (particle size 2 μm, i.d. 2 mm, length 100 mm) with a photodiode-array detector. The limits of detection and quantification of the UHPLC analyses were 0.09 and 0.29 mg/kg for delphinidin, 0.08 and 0.24 mg/kg for cyanidin, 0.09 and 0.26 mg/kg for petunidin, 0.14 and 0.42 mg/kg for pelargonidin, 0.16 and 0.48 mg/kg for peonidin and 0.30 and 0.91 mg/kg for malvidin, respectively. The intra- and inter-day precisions of individual anthocyanidin aglycones were <10.3%. All calibration curves exhibited good linearity (r = 0.999) within the tested ranges. The total run time of UHPLC was 8 min. The simple preparation method with UHPLC detection in this study presented herein significantly improved the speed and the simplicity for preparation step of delphinidin, cyanidin, petunidin, pelargonidin, peonidin and malvidin in fruits. Especially, the UHPLC detection exhibited good resolution in spite of shorter run time about four times than conventional HPLC detection. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  4. Trace element analysis of soil type collected from the Manjung and central Perak

    NASA Astrophysics Data System (ADS)

    Azman, Muhammad Azfar; Hamzah, Suhaimi; Rahman, Shamsiah Abdul; Elias, Md Suhaimi; Abdullah, Nazaratul Ashifa; Hashim, Azian; Shukor, Shakirah Abd; Kamaruddin, Ahmad Hasnulhadi Che

    2015-04-01

    Trace elements in soils primarily originated from their parent materials. Parents' material is the underlying geological material that has been undergone different types of chemical weathering and leaching processes. Soil trace elements concentrations may be increases as a result of continuous input from various human activities, including power generation, agriculture, mining and manufacturing. This paper describes the Neutron Activation Analysis (NAA) method used for the determination of trace elements concentrations in part per million (ppm) present in the terrestrial environment soil in Perak. The data may indicate any contamination of trace elements contributed from human activities in the area. The enrichment factors were used to check if there any contamination due to the human activities (power plants, agricultural, mining, etc.) otherwise the values would serve as a baseline data for future study. The samples were collected from 27 locations of different soil series in the area at two different depths: the top soil (0-15cm) and the sub soil (15-30cm). The collected soil samples were air dried at 60°C and passed through 2 µm sieve. Instrumental Neutron Activation Analysis (NAA) has been used for the determination of trace elements. Samples were activated in the Nuclear Malaysia TRIGA Mark II reactor followed by gamma spectrometric analysis. By activating the stable elements in the samples, the elements can be determined from the intensities of gamma energies emitted by the respected radionuclides.

  5. Trace element analysis of soil type collected from the Manjung and central Perak

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

    Azman, Muhammad Azfar, E-mail: m-azfar@nuclearmalaysia.gov.my; Hamzah, Suhaimi; Rahman, Shamsiah Abdul

    2015-04-29

    Trace elements in soils primarily originated from their parent materials. Parents’ material is the underlying geological material that has been undergone different types of chemical weathering and leaching processes. Soil trace elements concentrations may be increases as a result of continuous input from various human activities, including power generation, agriculture, mining and manufacturing. This paper describes the Neutron Activation Analysis (NAA) method used for the determination of trace elements concentrations in part per million (ppm) present in the terrestrial environment soil in Perak. The data may indicate any contamination of trace elements contributed from human activities in the area. Themore » enrichment factors were used to check if there any contamination due to the human activities (power plants, agricultural, mining, etc.) otherwise the values would serve as a baseline data for future study. The samples were collected from 27 locations of different soil series in the area at two different depths: the top soil (0-15cm) and the sub soil (15-30cm). The collected soil samples were air dried at 60°C and passed through 2 µm sieve. Instrumental Neutron Activation Analysis (NAA) has been used for the determination of trace elements. Samples were activated in the Nuclear Malaysia TRIGA Mark II reactor followed by gamma spectrometric analysis. By activating the stable elements in the samples, the elements can be determined from the intensities of gamma energies emitted by the respected radionuclides.« less

  6. Ultra-cold 4He atom beams

    NASA Astrophysics Data System (ADS)

    Mulders, N.; Wyatt, A. F. G.

    1994-02-01

    It has been shown that it is possible to create ultra-cold 4He atom beams, using a metal film heater covered with a superfluid helium film. The transient behaviour of the atom pulse can be improved significantly by shaping of the heater pulse. The leading edge of more energetic atoms can be suppressed nearly completely, leaving a core of mono-energetic atoms. The maximum number of atoms in the pulse is determined by the amount of helium in the superfluid film on the heater. This seriously limits the ranges of pulse width and energy over which this beam source can be operated. However, these can be increased significantly by using porous gold smoke heaters.

  7. Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples.

    PubMed

    Taher, Mohammad Ali; Pourmohammad, Fatemeh; Fazelirad, Hamid

    2015-12-01

    In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra-trace amounts of rhodium after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015-0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Profiles of non-essential trace elements in ewe and goat milk and their yoghurt, Torba yoghurt and whey.

    PubMed

    Sanal, Hasan; Güler, Zehra; Park, Young W

    2011-01-01

    The objectives of this study were to determine the profiles of non-essential trace elements in ewes' and goats' milk and manufactured products, such as yoghurt, torba yoghurt and whey, as well as changes in trace element content during Torba yoghurt-making processes. Concentrations of non-essential trace elements in ewe (Awassi) and goat (Damascus) milk and their yoghurt, torba yoghurt and whey were quantitatively determined by simultaneous inductively coupled plasma optical emission spectrometer (ICP-OES), after microwave digestion. Aluminium, antimony, arsenic, boron, beryllium, cadmium, nickel, lead, silver, titanium, thallium and vanadium were determined for both types of milk and their products. Barium was not detected in goats' milk or their products. Among all trace elements, boron was the most abundant and beryllium was least present in milk and the manufactured products. The results showed that goats' and ewes' milk and their manufactured products may be a source of 13 non-essential trace elements.

  9. Multi-ingredients determination and fingerprint analysis of leaves from Ilex latifolia using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry.

    PubMed

    Fan, Chunlin; Deng, Jiewei; Yang, Yunyun; Liu, Junshan; Wang, Ying; Zhang, Xiaoqi; Fai, Kuokchiu; Zhang, Qingwen; Ye, Wencai

    2013-10-01

    An ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) method integrating multi-ingredients determination and fingerprint analysis has been established for quality assessment and control of leaves from Ilex latifolia. The method possesses the advantages of speediness, efficiency, accuracy, and allows the multi-ingredients determination and fingerprint analysis in one chromatographic run within 13min. Multi-ingredients determination was performed based on the extracted ion chromatograms of the exact pseudo-molecular ions (with a 0.01Da window), and fingerprint analysis was performed based on the base peak chromatograms, obtained by negative-ion electrospray ionization QTOF-MS. The method validation results demonstrated our developed method possessing desirable specificity, linearity, precision and accuracy. The method was utilized to analyze 22 I. latifolia samples from different origins. The quality assessment was achieved by using both similarity analysis (SA) and principal component analysis (PCA), and the results from SA were consistent with those from PCA. Our experimental results demonstrate that the strategy integrated multi-ingredients determination and fingerprint analysis using UPLC-QTOF-MS technique is a useful approach for rapid pharmaceutical analysis, with promising prospects for the differentiation of origin, the determination of authenticity, and the overall quality assessment of herbal medicines. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Trace-element concentrations in streambed sediment across the conterminous United States

    USGS Publications Warehouse

    Rice, Karen C.

    1999-01-01

    Trace-element concentrations in 541 streambed-sediment samples collected from 20 study areas across the conterminous United States were examined as part of the National Water-Quality Assessment Program of the U.S. Geological Survey. Sediment samples were sieved and the <63-μm fraction was retained for determination of total concentrations of trace elements. Aluminum, iron, titanium, and organic carbon were weakly or not at all correlated with the nine trace elements examined:  arsenic, cadmium, chromium, copper, lead, mercury, nickel, selenium, and zinc. Four different methods of accounting for background/baseline concentrations were examined; however, normalization was not required because field sieving removed most of the background differences between samples. The sum of concentrations of trace elements characteristic of urban settings - copper, mercury, lead, and zinc - was well correlated with population density, nationwide. Median concentrations of seven trace elements (all nine examined except arsenic and selenium) were enriched in samples collected from urban settings relative to agricultural or forested settings. Forty-nine percent of the sites sampled in urban settings had concentrations of one or more trace elements that exceeded levels at which adverse biological effects could occur in aquatic biota.

  11. Preliminary Analysis of the 30-m UltraBoom Flight Test

    NASA Technical Reports Server (NTRS)

    Agnes, Gregory S.; Abelson, Robert D.; Miyake, Robert; Lin, John K. H.; Welsh, Joe; Watson, Judith J.

    2005-01-01

    Future NASA missions require long, ultra-lightweight booms to enable solar sails, large sunshields, and other gossamer-type spacecraft structures. The space experiment discussed in this paper will flight validate the non-traditional ultra lightweight rigidizable, inflatable, isogrid structure utilizing graphite shape memory polymer (GR/SMP) called UltraBoom(TradeMark). The focus of this paper is the analysis of the 3-m ground test article. The primary objective of the mission is to show that a combination of ground testing and analysis can predict the on-orbit performance of an ultra lightweight boom that is scalable, predictable, and thermomechanically stable.

  12. A simple and rapid ultra-high-performance liquid chromatography-tandem mass spectrometry method to determine plasma biotin in hemodialysis patients.

    PubMed

    Yagi, Shigeaki; Nishizawa, Manabu; Ando, Itiro; Oguma, Shiro; Sato, Emiko; Imai, Yutaka; Fujiwara, Masako

    2016-08-01

    A simple, rapid, and selective method for determination of plasma biotin was developed using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). After single-step protein precipitation with methanol, biotin and stable isotope-labeled biotin as an internal standard (IS) were chromatographed on a pentafluorophenyl stationary-phase column (2.1 × 100 mm, 2.7 μm) under isocratic conditions using 10 mm ammonium formate-acetonitrile (93:7, v/v) at a flow rate of 0.6 mL/min. The total chromatographic runtime was 5 min for each injection. Detection was performed in a positive electrospray ionization mode by monitoring selected ion transitions at m/z 245.1/227.0 and 249.1/231.0 for biotin and the IS, respectively. The calibration curve was linear in the range of 0.05-2 ng/mL using 300 μL of plasma. The intra- and inter-day precisions were all <7.1%. The accuracy varied from -0.7 to 8.2%. The developed UHPLC-MS/MS method was successfully applied to determine plasma biotin concentrations in hemodialysis patients. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  13. Simultaneous determination of bisphenols and alkylphenols in water by solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Shan, Xiao Mei; Shen, Deng Hui; Wang, Bing Shuang; Lu, Bei Bei; Huang, Fa Yuan

    2014-06-01

    To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0 μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%. Relative standard deviations (RSDs) were between 1.26% and 3.67%. Applying this method to detect the source water of Chaohu Lake and drinking water of Hefei, six target compounds were detected in different levels. This method is simple with high sensitivity and selectivity, could be suitable for the determination of these compounds in source and drinking water. Copyright © 2014 The Editorial Board of Biomedical and Environmental Sciences. Published by China CDC. All rights reserved.

  14. Determination of rutin in rat plasma by ultra performance liquid chromatography tandem mass spectrometry and application to pharmacokinetic study.

    PubMed

    Chen, Mengchun; Zhang, Xiaoqian; Wang, Hao; Lin, Baoli; Wang, Shuanghu; Hu, Guoxin

    2015-04-01

    A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) method for the determination of rutin in rat plasma was developed and validated. After addition of tolbutamide as internal standard (IS), protein precipitation by acetonitrile was used as sample preparation. The chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm particle size), using acetonitrile-0.1% formic acid as the mobile phase with gradient elution, delivered at a flow-rate of 0.4 mL/min. Mass spectrometric analysis was performed using a XEVO TQD mass spectrometer coupled with an electro-spray ionization (ESI) source in the positive ion mode. The MRM transitions of m/z 610.91→302.98 and m/z 271.2→155.1 were used to quantify for rutin and tolbutamide, respectively. This assay method has been fully validated in terms of specificity, linearity, recovery and matrix effect, accuracy, precision and stability. Calibration curves were linear in the concentration ranges of 25-2000 ng/mL for rutin. Only 3 min was needed for an analytical run. This developed method was successfully used for determination of rutin in rat plasma for pharmacokinetic study. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  15. Major to ultra trace element bulk rock analysis of nanoparticulate pressed powder pellets by LA-ICP-MS

    NASA Astrophysics Data System (ADS)

    Peters, Daniel; Pettke, Thomas

    2016-04-01

    An efficient, clean procedure for bulk rock major to trace element analysis by 193 nm Excimer LA-ICP-MS analysis of nanoparticulate pressed powder pellets (PPPs) employing a binder is presented. Sample powders are milled in water suspension in a planetary ball mill, reducing average grain size by about one order of magnitude compared to common dry milling protocols. Microcrystalline cellulose (MCC) is employed as a binder, improving the mechanical strength of the PPP and the ablation behaviour, because MCC absorbs 193 nm laser light well. Use of MCC binder allows for producing cohesive pellets of materials that cannot be pelletized in their pure forms, such as quartz powder. Rigorous blank quantification was performed on synthetic quartz treated like rock samples, demonstrating that procedural blanks are irrelevant except for a few elements at the 10 ng g-1 concentration level. The LA-ICP-MS PPP analytical procedure was optimised and evaluated using six different SRM powders (JP-1, UB-N, BCR-2, GSP-2, OKUM, and MUH-1). Calibration based on external standardization using SRM 610, SRM 612, BCR-2G, and GSD-1G glasses allows for evaluation of possible matrix effects during LA-ICP-MS analysis. The data accuracy of the PPP LA-ICP-MS analytical procedure compares well to that achieved for liquid ICP-MS and LA-ICP-MS glass analysis, except for element concentrations below ˜30 ng g-1, where liquid ICP-MS offers more precise data and in part lower limits of detection. Uncertainties on the external reproducibility of LA-ICP-MS PPP element concentrations are of the order of 0.5 to 2 % (1σ standard deviation) for concentrations exceeding ˜1 μg g-1. For lower element concentrations these uncertainties increase to 5-10% or higher when analyte-depending limits of detection (LOD) are approached, and LODs do not significantly differ from glass analysis. Sample homogeneity is demonstrated by the high analytical precision, except for very few elements where grain size effects can

  16. Light-curve and spectral properties of ultra-stripped core-collapse supernovae

    NASA Astrophysics Data System (ADS)

    Moriya, Takashi J.

    2017-11-01

    We discuss light-curve and spectral properties of ultra-stripped core-collapse supernovae. Ultra-stripped supernovae are supernovae with ejecta masses of only ~0.1M ⊙ whose progenitors lose their envelopes due to binary interactions with their compact companion stars. We follow the evolution of an ultra-stripped supernova progenitor until core collapse and perform explosive nucleosynthesis calculations. We then synthesize light curves and spectra of ultra-stripped supernovae based on the nucleosynthesis results. We show that ultra-stripped supernovae synthesize ~0.01M ⊙ of the radioactive 56Ni, and their typical peak luminosity is around 1042 erg s-1 or -16 mag. Their typical rise time is 5 - 10 days. By comparing synthesized and observed spectra, we find that SN 2005ek and some of so-called calcium-rich gap transients like PTF10iuv may be related to ultra-stripped supernovae.

  17. [Contents of ten trace elements in Epimedium acuminatum Franch. and its different processed products].

    PubMed

    Chen, H L; Wang, J K; Ren, Y Q; Wu, Z Y

    2001-03-01

    Determine and compare the contents of ten trace elements in crude E. acuminatum and its three different processed products. Using flame atomic absorption spectrometry. The ten trace elements were found in both the crude drug and its three processed products, and in terms of contents some of the trace elements in all the three processed products are higher than those in the crude drug. According to the trace element contents, the three processed products of E. acuminatum have their own advantages. It is thus suggested that thoroughgoing clinical and experimental researches be performed anew for the long-shelved processing methods.

  18. Selective and sensitized spectrophotometric determination of trace amounts of Ni(II) ion using α-benzyl dioxime in surfactant media

    NASA Astrophysics Data System (ADS)

    Ghaedi, Mehrorang

    2007-02-01

    Highly sensitive and interference-free sensitized spectrophotometric method for the determination of Ni(II) ions is described. The method is based on the reaction between Ni(II) ion and benzyl dioxime in micellar media in the presence of sodium dodecyl sulfate (SDS). The absorbance is linear from 0.1 up to 25.0 μg mL -1 in aqueous solution with repeatability (RSD) of 1.0% at a concentration of 1 μg mL -1 and a detection limit of 0.12 ng mL -1 and molar absorption coefficient of 68,600 L mol -1 cm -1. The influence of reaction variables including type and amount of surfactant, pH, and amount of ligand and complexation time and the effect of interfering ions are investigated. The proposed procedure was applied to the determination of trace amounts of Ni(II) ion in tap water, river water, chocolate and vegetable without separation or organic solvent extraction.

  19. Determination of colistin in animal tissues, egg, milk, and feed by ultra-high performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Fu, Qin; Li, Xiaowei; Zheng, Kangni; Ke, Yuebin; Wang, Yingyu; Wang, Lina; Yu, Fugen; Xia, Xi

    2018-05-15

    A confirmatory method for the determination of colistin in animal tissues, egg, milk, and feed was developed and validated. Colistin A and colistin B were extracted from samples with the mixture of 10% trichloroacetic acid-acetonitrile and isolated with mixed-mode weak cation exchange cartridge. Analytes were separated from matrix components using ultra-high performance liquid chromatography, and detected with electrospray ionization on a triple quadrupole mass spectrometer. Mean recoveries ranged from 78.0% to 115.6% with intra-day and inter-day relative standard deviation lower than 8.4% and 12.4%, respectively. The quantitation limits for different matrices were between 5 and 30 μg/kg, which was satisfactory for surveillance monitoring. The developed method was applied to the analysis of real samples collected from different provinces of China, and 19 out of 348 samples were found to be contaminated, with the highest concentration of approximately 12,000 μg/kg colistin A and 10,000 μg/kg colistin B in feed. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. New method to determine the refractive index and the absorption coefficient of organic nonlinear crystals in the ultra-wideband THz region.

    PubMed

    Ohno, Seigo; Miyamoto, Katsuhiko; Minamide, Hiroaki; Ito, Hiromasa

    2010-08-02

    A method for simultaneously measuring the refractive index and absorption coefficient of nonlinear optical crystals in the ultra-wideband terahertz (THz) region is described. This method is based on the analysis of a collinear difference frequency generation (DFG) process using a tunable, dual-wavelength, optical parametric oscillator. The refractive index and the absorption coefficient in the organic nonlinear crystal DAST were experimentally determined in the frequency range 2.5-26.2 THz by measuring the THz-wave output using DFG. The resultant refractive index in the x-direction was approximately 2.3, while the absorption spectrum was in good agreement with FT-IR measurements. The output of the DAST-DFG THz-wave source was optimized to the phase-matching condition using the measured refractive index spectrum in THz region, which resulted in an improvement in the output power of up to a factor of nine.

  1. Ultra-Sensitive Elemental Analysis Using Plasmas 7.Application to Criminal Investigation

    NASA Astrophysics Data System (ADS)

    Suzuki, Yasuhiro

    This paper describes the application of trace elemental analysis using ICP-AES and ICP-MS to criminal investigation. The comparison of trace elements, such as Rb, Sr, Zr, and so on, is effective for the forensic discrimination of glass fragments, which can be important physical evidence for connecting a suspect to a crime scene or to a victim. This procedure can be applied also to lead shotgun pellets by the removal of matrix lead as the sulfate precipitate after the dissolution of a pellet sample. The determination of a toxic element in bio-logical samples is required to prove that a victim ingested this element. Arsenous acids produced in Japan, China, Germany and Switzerland show characteristic patterns of trace elements characteristic to each country.

  2. Predicting Individual Characteristics from Digital Traces on Social Media: A Meta-Analysis.

    PubMed

    Settanni, Michele; Azucar, Danny; Marengo, Davide

    2018-04-01

    The increasing utilization of social media provides a vast and new source of user-generated ecological data (digital traces), which can be automatically collected for research purposes. The availability of these data sets, combined with the convergence between social and computer sciences, has led researchers to develop automated methods to extract digital traces from social media and use them to predict individual psychological characteristics and behaviors. In this article, we reviewed the literature on this topic and conducted a series of meta-analyses to determine the strength of associations between digital traces and specific individual characteristics; personality, psychological well-being, and intelligence. Potential moderator effects were analyzed with respect to type of social media platform, type of digital traces examined, and study quality. Our findings indicate that digital traces from social media can be studied to assess and predict theoretically distant psychosocial characteristics with remarkable accuracy. Analysis of moderators indicated that the collection of specific types of information (i.e., user demographics), and the inclusion of different types of digital traces, could help improve the accuracy of predictions.

  3. Ultra-Short-Term Heart Rate Variability is Sensitive to Training Effects in Team Sports Players.

    PubMed

    Nakamura, Fabio Y; Flatt, Andrew A; Pereira, Lucas A; Ramirez-Campillo, Rodrigo; Loturco, Irineu; Esco, Michael R

    2015-09-01

    The aim of this study was to test the possibility of the ultra-short-term lnRMSSD (measured in 1-min post-1-min stabilization period) to detect training induced adaptations in futsal players. Twenty-four elite futsal players underwent HRV assessments pre- and post-three or four weeks preseason training. From the 10-min HRV recording period, lnRMSSD was analyzed in the following time segments: 1) from 0-5 min (i.e., stabilization period); 2) from 0-1 min; 1-2 min; 2-3 min; 3-4 min; 4-5 min and; 3) from 5-10 min (i.e., criterion period). The lnRMSSD was almost certainly higher (100/00/00) using the magnitude-based inference in all periods at the post- moment. The correlation between changes in ultra-short-term lnRMSSD (i.e., 0-1 min; 1-2 min; 2-3 min; 3-4 min; 4-5 min) and lnRMSSDCriterion ranged between 0.45-0.75, with the highest value (p = 0.75; 90% CI: 0.55 - 0.85) found between ultra-short-term lnRMDSSD at 1-2 min and lnRMSSDCriterion. In conclusion, lnRMSSD determined in a short period of 1-min is sensitive to training induced changes in futsal players (based on the very large correlation to the criterion measure), and can be used to track cardiac autonomic adaptations. Key pointsThe ultra-short-term (1 min) natural log of the root-mean-square difference of successive normal RR intervals (lnRMSSD) is sensitive to training effects in futsal playersThe ultra-short-term lnRMSSD may simplify the assessment of the cardiac autonomic changes in the field compared to the traditional and lengthier (10 min duration) analysisCoaches are encouraged to implement the ultra-short-term heart rate variability in their routines to monitor team sports athletes.

  4. Ultra-Short-Term Heart Rate Variability is Sensitive to Training Effects in Team Sports Players

    PubMed Central

    Nakamura, Fabio Y.; Flatt, Andrew A.; Pereira, Lucas A.; Ramirez-Campillo, Rodrigo; Loturco, Irineu; Esco, Michael R.

    2015-01-01

    The aim of this study was to test the possibility of the ultra-short-term lnRMSSD (measured in 1-min post-1-min stabilization period) to detect training induced adaptations in futsal players. Twenty-four elite futsal players underwent HRV assessments pre- and post-three or four weeks preseason training. From the 10-min HRV recording period, lnRMSSD was analyzed in the following time segments: 1) from 0-5 min (i.e., stabilization period); 2) from 0-1 min; 1-2 min; 2-3 min; 3-4 min; 4-5 min and; 3) from 5-10 min (i.e., criterion period). The lnRMSSD was almost certainly higher (100/00/00) using the magnitude-based inference in all periods at the post- moment. The correlation between changes in ultra-short-term lnRMSSD (i.e., 0-1 min; 1-2 min; 2-3 min; 3-4 min; 4-5 min) and lnRMSSDCriterion ranged between 0.45-0.75, with the highest value (p = 0.75; 90% CI: 0.55 – 0.85) found between ultra-short-term lnRMDSSD at 1-2 min and lnRMSSDCriterion. In conclusion, lnRMSSD determined in a short period of 1-min is sensitive to training induced changes in futsal players (based on the very large correlation to the criterion measure), and can be used to track cardiac autonomic adaptations. Key points The ultra-short-term (1 min) natural log of the root-mean-square difference of successive normal RR intervals (lnRMSSD) is sensitive to training effects in futsal players The ultra-short-term lnRMSSD may simplify the assessment of the cardiac autonomic changes in the field compared to the traditional and lengthier (10 min duration) analysis Coaches are encouraged to implement the ultra-short-term heart rate variability in their routines to monitor team sports athletes PMID:26336347

  5. Comparison of Cryopreserved Human Sperm between Ultra Rapid Freezing and Slow Programmable Freezing: Effect on Motility, Morphology and DNA Integrity.

    PubMed

    Tongdee, Pattama; Sukprasert, Matchuporn; Satirapod, Chonticha; Wongkularb, Anna; Choktanasiri, Wicham

    2015-05-01

    Cryopreservation of sperm is common methods to preserve male fertility. Sperm freezing, suggest slow programmable freezing caused lower change of sperm morphology than sperm freezing in vapor of liquid nitrogen. Ultra rapid freezing is easy to be worked on, less time, low cost and does not need high experience. To compare the effect on sperm motility, morphology and DNA integrity of post-thawed sperm after ultra rapid freezing and slow programmable freezing methods. Experimental study at laboratory of infertility unit, Department of Obstetrics and Gynecology, Faculty of Medicine Ramathibodi Hospital. Thirty-seven semen samples with normal semen analysis according to World Health Organization (WHO) 1999 [normal sperm volume ( 2 ml) and normal sperm concentration (≥ 20 x10(6)/ml) and sperm motility (≥ 50%)]. Semen samples were washed. Then each semen sample was divided into six cryovials. Two cryovials, 0.5 ml each, were cryopreserved by slow programmable freezing. Four 0.25 ml containing cryovials, were cryopreserved by ultra rapidfreezing method. After cryopreservationfor 1 month, thawedprocess was carried out at room temperature. Main outcomes are sperm motility was determined by Computer-Assisted Semen Analysis (CASA), sperm morphology was determined by eosin-methylene blue staining and sperm DNA integrity was assessed by TUNEL assay. Sperm motility was reduced significantly by both methods, from 70.4 (9.0)% to 29.1 (12.3)% in slowprogrammable freezing and to 19.7 (9.8)% in ultra rapid freezing (p < 0.05). Sperm motility decreased significantly more by ultra rapid freezing (p < 0.001). The percentage of normal sperm morphology and DNA integrity were also reduced significantly by both methods. However, no significant difference between the two methods was found (p > 0.05). Cryopreservation of human sperm for 1 month significantly decreased sperm motility, morphology and DNA integrity in both methods. However sperm motility was decreased more by ultra rapid

  6. New approach to the determination phosphorothioate oligonucleotides by ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry.

    PubMed

    Studzińska, Sylwia; Mounicou, Sandra; Szpunar, Joanna; Łobiński, Ryszard; Buszewski, Bogusław

    2015-01-15

    This text presents a novel method for the separation and detection of phosphorothioate oligonucleotides with the use of ion pair ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry The research showed that hexafluoroisopropanol/triethylamine based mobile phases may be successfully used when liquid chromatography is coupled with such elemental detection. However, the concentration of both HFIP and TEA influences the final result. The lower concentration of HFIP, the lower the background in ICP-MS and the greater the sensitivity. The method applied for the analysis of serum samples was based on high resolution inductively coupled plasma mass spectrometry. Utilization of this method allows determination of fifty times lower quantity of phosphorothioate oligonucleotides than in the case of quadrupole mass analyzer. Monitoring of (31)P may be used to quantify these compounds at the level of 80 μg L(-1), while simultaneous determination of sulfur is very useful for qualitative analysis. Moreover, the results presented in this paper demonstrate the practical applicability of coupling LC with ICP-MS in determining phosphorothioate oligonucleotides and their metabolites in serum within 7 min with a very good sensitivity. The method was linear in the concentration range between 0.2 and 3 mg L(-1). The limit of detection was in the range of 0.07 and 0.13 mg L(-1). Accuracy varied with concentration, but was in the range of 3%. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Determination of fluorine by total reflection X-ray fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Tarsoly, G.; Óvári, M.; Záray, Gy.

    2010-04-01

    There is a growing interest in determination of low Z elements, i.e. carbon to phosphorus, in various samples. Total reflection X-ray fluorescence spectrometry (TXRF) has been already established as a suitable trace element analytical method with low sample demand and quite good quantification limits. Recently, the determinable element range was extended towards Z = 6 (carbon). In this study, the analytical performance of the total reflection X-ray fluorescence spectrometry for determination of fluorine was investigated applying a spectrometer equipped with Cr-anode X-ray tube, multilayer monochromator, vacuum chamber, and a silicon drift detector (SDD) with ultra thin window was used. The detection limit for fluorine was found to be 5 mg L - 1 (equivalent to 10 ng absolute) in aqueous matrix. The linear range of the fluorine determination is between 15 and 500 mg L - 1 , within this range the precision is below 10%. The matrix effects of the other halogens (chlorine, bromine and iodine), and sulfate were also investigated. It has been established that the upper allowed concentration limit of the above interfering elements is 100, 200, 50 and 100 mg L - 1 for Cl, Br, I and sulfate, respectively. Moreover, the role of the pre-siliconization of the quartz carrier plate was investigated. It was found, that the presence of the silicone results in poorer analytical performance, which can be explained by the thicker sample residue and stronger self-absorption of the fluorescent radiation.

  8. Quantile Regression for Analyzing Heterogeneity in Ultra-high Dimension

    PubMed Central

    Wang, Lan; Wu, Yichao

    2012-01-01

    Ultra-high dimensional data often display heterogeneity due to either heteroscedastic variance or other forms of non-location-scale covariate effects. To accommodate heterogeneity, we advocate a more general interpretation of sparsity which assumes that only a small number of covariates influence the conditional distribution of the response variable given all candidate covariates; however, the sets of relevant covariates may differ when we consider different segments of the conditional distribution. In this framework, we investigate the methodology and theory of nonconvex penalized quantile regression in ultra-high dimension. The proposed approach has two distinctive features: (1) it enables us to explore the entire conditional distribution of the response variable given the ultra-high dimensional covariates and provides a more realistic picture of the sparsity pattern; (2) it requires substantially weaker conditions compared with alternative methods in the literature; thus, it greatly alleviates the difficulty of model checking in the ultra-high dimension. In theoretic development, it is challenging to deal with both the nonsmooth loss function and the nonconvex penalty function in ultra-high dimensional parameter space. We introduce a novel sufficient optimality condition which relies on a convex differencing representation of the penalized loss function and the subdifferential calculus. Exploring this optimality condition enables us to establish the oracle property for sparse quantile regression in the ultra-high dimension under relaxed conditions. The proposed method greatly enhances existing tools for ultra-high dimensional data analysis. Monte Carlo simulations demonstrate the usefulness of the proposed procedure. The real data example we analyzed demonstrates that the new approach reveals substantially more information compared with alternative methods. PMID:23082036

  9. On the maximum energy of shock-accelerated cosmic rays at ultra-relativistic shocks

    NASA Astrophysics Data System (ADS)

    Reville, B.; Bell, A. R.

    2014-04-01

    The maximum energy to which cosmic rays can be accelerated at weakly magnetised ultra-relativistic shocks is investigated. We demonstrate that for such shocks, in which the scattering of energetic particles is mediated exclusively by ion skin-depth scale structures, as might be expected for a Weibel-mediated shock, there is an intrinsic limit on the maximum energy to which particles can be accelerated. This maximum energy is determined from the requirement that particles must be isotropized in the downstream plasma frame before the mean field transports them far downstream, and falls considerably short of what is required to produce ultra-high-energy cosmic rays. To circumvent this limit, a highly disorganized field is required on larger scales. The growth of cosmic ray-induced instabilities on wavelengths much longer than the ion-plasma skin depth, both upstream and downstream of the shock, is considered. While these instabilities may play an important role in magnetic field amplification at relativistic shocks, on scales comparable to the gyroradius of the most energetic particles, the calculated growth rates have insufficient time to modify the scattering. Since strong modification is a necessary condition for particles in the downstream region to re-cross the shock, in the absence of an alternative scattering mechanism, these results imply that acceleration to higher energies is ruled out. If weakly magnetized ultra-relativistic shocks are disfavoured as high-energy particle accelerators in general, the search for potential sources of ultra-high-energy cosmic rays can be narrowed.

  10. Measurement of trace nitrate concentrations in seawater by ion chromatography with valve switching

    NASA Astrophysics Data System (ADS)

    Du, Juan; Fa, Yun; Zheng, Yue; Li, Xuebing; Du, Fanglin; Yang, Haiyan

    2014-05-01

    An ion chromatographic method with a valve switching facility was developed to determine trace nitrate concentrations in seawater using two pumps, two different suppressors, and two columns. A carbohydrate membrane desalter was used to reduce the high concentrations of sodium salts in samples. In this method, trace nitrate was eluted from the concentrator column to the analytical columns, while the matrix fl owed to waste. Neither chemical pre-treatment nor sample dilution was required. In the optimized separation conditions, the method showed good linearity ( R >0.99) in the 0.05 and 50 mg/L concentration range, and satisfactory repeatability (RSD<5%, n =6). The limit of detection for nitrate was 0.02 mg/L. Results showed that the valve switching system was suitable and practical for the determination of trace nitrate in seawater.

  11. Ultra-thin plasma panel radiation detector

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

    Friedman, Peter S.

    An ultra-thin radiation detector includes a radiation detector gas chamber having at least one ultra-thin chamber window and an ultra-thin first substrate contained within the gas chamber. The detector further includes a second substrate generally parallel to and coupled to the first substrate and defining a gas gap between the first substrate and the second substrate. The detector further includes a discharge gas between the substrates and contained within the gas chamber, where the discharge gas is free to circulate within the gas chamber and between the first and second substrates at a given gas pressure. The detector further includesmore » a first electrode coupled to one of the substrates and a second electrode electrically coupled to the first electrode. The detector further includes a first discharge event detector coupled to at least one of the electrodes for detecting a gas discharge counting event in the electrode.« less

  12. Different rates of spontaneous mutation of chloroplastic and nuclear viroids as determined by high-fidelity ultra-deep sequencing.

    PubMed

    López-Carrasco, Amparo; Ballesteros, Cristina; Sentandreu, Vicente; Delgado, Sonia; Gago-Zachert, Selma; Flores, Ricardo; Sanjuán, Rafael

    2017-09-01

    Mutation rates vary by orders of magnitude across biological systems, being higher for simpler genomes. The simplest known genomes correspond to viroids, subviral plant replicons constituted by circular non-coding RNAs of few hundred bases. Previous work has revealed an extremely high mutation rate for chrysanthemum chlorotic mottle viroid, a chloroplast-replicating viroid. However, whether this is a general feature of viroids remains unclear. Here, we have used high-fidelity ultra-deep sequencing to determine the mutation rate in a common host (eggplant) of two viroids, each representative of one family: the chloroplastic eggplant latent viroid (ELVd, Avsunviroidae) and the nuclear potato spindle tuber viroid (PSTVd, Pospiviroidae). This revealed higher mutation frequencies in ELVd than in PSTVd, as well as marked differences in the types of mutations produced. Rates of spontaneous mutation, quantified in vivo using the lethal mutation method, ranged from 1/1000 to 1/800 for ELVd and from 1/7000 to 1/3800 for PSTVd depending on sequencing run. These results suggest that extremely high mutability is a common feature of chloroplastic viroids, whereas the mutation rates of PSTVd and potentially other nuclear viroids appear significantly lower and closer to those of some RNA viruses.

  13. Pilot projects for improving product tracing along the food supply system.

    PubMed

    Bhatt, Tejas; Hickey, Caitlin; McEntire, Jennifer C

    2013-12-01

    In September 2011, the U.S. Food and Drug Administration (FDA) asked the Institute of Food Technologists (IFT) to execute product tracing pilot projects as described in Section 204 of the FDA Food Safety Modernization Act (FSMA). IFT collaborated with representatives from more than 100 organizations-including the U.S. Dept. of Agriculture, state departments of agriculture and public health, industry, and consumer groups, as well as not-for-profit organizations-to implement the pilots. The objectives of the pilot projects were 1) to identify and gather information on methods to improve product tracing of foods in the supply chain and 2) to explore and evaluate methods to rapidly and effectively identify the recipient of food to prevent or mitigate a foodborne illness outbreak and to address credible threats of serious adverse health consequences or death to humans or animals as a result of such food being adulterated or misbranded. IFT conducted evaluations to determine the impact of currently available technologies, types of data and formats, and the data acquisition process, as well as the use of technology on the ability to follow product movement through the supply chain. Results from the pilots found inconsistencies in the terminology, numbering systems, formatting, legibility, and occasionally the language that sometimes required IFT to contact the submitting firm to gain clarity, thus increasing the time required to capture data before any meaningful analysis could begin. However, the pilot participants appeared to have many of the tools and processes in place which are required to allow the capture and communication of critical track and trace information (such as, key data elements) at critical points of product transfer and transformation (such as, critical tracking events). IFT determined that costs associated with implementing a product tracing system can vary widely as determined by numerous factors: the size of the firm/facility, the method of product

  14. The role of the seagrass Posidonia oceanica in the cycling of trace elements

    NASA Astrophysics Data System (ADS)

    Sanz-Lázaro, C.; Malea, P.; Apostolaki, E. T.; Kalantzi, I.; Marín, A.; Karakassis, I.

    2012-03-01

    The aim of this work was to study the role of the seagrass Posidonia oceanica on the cycling of a wide set of trace elements (Ag, As, Ba, Bi, Cd, Co, Cr, Cs, Cu, Fe, Ga, Li, Mn, Ni, Pb, Rb, Sr, Tl, V and Zn). We measured the concentration of these trace elements in the different compartments of P. oceanica (leaves, rhizomes, roots and epibiota) in a non-polluted seagrass meadow representative of the Mediterranean and calculated the annual budget from a mass balance. We provide novel data on accumulation dynamics of many trace elements in P. oceanica compartments and demonstrate that trace element accumulation patterns are mainly determined by plant compartment rather than by temporal variability. Epibiota was the compartment which showed the greatest concentrations for most trace elements. Thus, they constitute a key compartment when estimating trace element transfer to higher trophic levels by P. oceanica. For most trace elements, translocation seemed to be low and acropetal. Zn, Cd, Sr and Rb were the trace elements that showed the highest release rate through decomposition of plant detritus, while Cs, Tl and Bi the lowest. P. oceanica acts as a sink of potentially toxic trace elements (Ni, Cr, As and Ag), which can be sequestered, decreasing their bioavailability. P. oceanica may have a relevant role in the cycling of trace elements in the Mediterranean.

  15. The role of the seagrass Posidonia oceanica in the cycling of trace elements

    NASA Astrophysics Data System (ADS)

    Sanz-Lázaro, C.; Malea, P.; Apostolaki, E. T.; Kalantzi, I.; Marín, A.; Karakassis, I.

    2012-07-01

    The aim of this study was to investigate the role of the seagrass Posidonia oceanica on the cycling of a wide set of trace elements (Ag, As, Ba, Bi, Cd, Co, Cr, Cs, Cu, Fe, Ga, Li, Mn, Ni, Pb, Rb, Sr, Tl, V and Zn). We measured the concentration of these trace elements in different compartments of P. oceanica (leaves, rhizomes, roots and epiphytes) in a non-polluted seagrass meadow representative of the Mediterranean and calculated the annual budget from a mass balance. We provide novel data on accumulation dynamics of many trace elements in P. oceanica compartments and demonstrate that trace element accumulation patterns are mainly determined by plant compartment rather than by temporal variability. Epiphytes were the compartment, which showed the greatest concentrations for most trace elements. Thus, they constitute a key compartment when estimating trace element transfer to higher trophic levels by P. oceanica. Trace element translocation in P. oceanica seemed to be low and acropetal in most cases. Zn, Cd, Sr and Rb were the trace elements that showed the highest release rate through decomposition of plant detritus, while Cs, Tl and Bi showed the lowest. P. oceanica acts as a sink of potentially toxic trace elements (Ni, Cr, As and Ag), which can be sequestered, decreasing their bioavailability. P. oceanica may have a relevant role in the cycling of trace elements in the Mediterranean.

  16. Training-Dependent Associative Learning Induced Neocortical Structural Plasticity: A Trace Eyeblink Conditioning Analysis

    PubMed Central

    Chau, Lily S.; Prakapenka, Alesia V.; Zendeli, Liridon; Davis, Ashley S.; Galvez, Roberto

    2014-01-01

    Studies utilizing general learning and memory tasks have suggested the importance of neocortical structural plasticity for memory consolidation. However, these learning tasks typically result in learning of multiple different tasks over several days of training, making it difficult to determine the synaptic time course mediating each learning event. The current study used trace-eyeblink conditioning to determine the time course for neocortical spine modification during learning. With eyeblink conditioning, subjects are presented with a neutral, conditioned stimulus (CS) paired with a salient, unconditioned stimulus (US) to elicit an unconditioned response (UR). With multiple CS-US pairings, subjects learn to associate the CS with the US and exhibit a conditioned response (CR) when presented with the CS. Trace conditioning is when there is a stimulus free interval between the CS and the US. Utilizing trace-eyeblink conditioning with whisker stimulation as the CS (whisker-trace-eyeblink: WTEB), previous findings have shown that primary somatosensory (barrel) cortex is required for both acquisition and retention of the trace-association. Additionally, prior findings demonstrated that WTEB acquisition results in an expansion of the cytochrome oxidase whisker representation and synaptic modification in layer IV of barrel cortex. To further explore these findings and determine the time course for neocortical learning-induced spine modification, the present study utilized WTEB conditioning to examine Golgi-Cox stained neurons in layer IV of barrel cortex. Findings from this study demonstrated a training-dependent spine proliferation in layer IV of barrel cortex during trace associative learning. Furthermore, findings from this study showing that filopodia-like spines exhibited a similar pattern to the overall spine density further suggests that reorganization of synaptic contacts set the foundation for learning-induced neocortical modifications through the different

  17. Address tracing for parallel machines

    NASA Technical Reports Server (NTRS)

    Stunkel, Craig B.; Janssens, Bob; Fuchs, W. Kent

    1991-01-01

    Recently implemented parallel system address-tracing methods based on several metrics are surveyed. The issues specific to collection of traces for both shared and distributed memory parallel computers are highlighted. Five general categories of address-trace collection methods are examined: hardware-captured, interrupt-based, simulation-based, altered microcode-based, and instrumented program-based traces. The problems unique to shared memory and distributed memory multiprocessors are examined separately.

  18. SolTrace | Concentrating Solar Power | NREL

    Science.gov Websites

    NREL packaged distribution or from source code at the SolTrace open source project website. NREL Publications Support FAQs SolTrace open source project The code uses Monte-Carlo ray-tracing methodology. The -tracing capabilities. With the release of the SolTrace open source project, the software has adopted

  19. Note: A dual temperature closed loop batch reactor for determining the partitioning of trace gases within CO2-water systems.

    PubMed

    Warr, Oliver; Rochelle, Christopher A; Masters, Andrew J; Ballentine, Christopher J

    2016-01-01

    An experimental approach is presented which can be used to determine partitioning of trace gases within CO2-water systems. The key advantages of this system are (1) The system can be isolated with no external exchange, making it ideal for experiments with conservative tracers. (2) Both phases can be sampled concurrently to give an accurate composition at each phase at any given time. (3) Use of a lower temperature flow loop outside of the reactor removes contamination and facilitates sampling. (4) Rapid equilibration at given pressure/temperature conditions is significantly aided by stirring and circulating the water phase using a magnetic stirrer and high-pressure liquid chromatography pump, respectively.

  20. Ultra-Fast Microwave Synthesis of ZnO Nanorods on Cellulose Substrates for UV Sensor Applications

    PubMed Central

    Pimentel, Ana; Samouco, Ana; Araújo, Andreia; Martins, Rodrigo; Fortunato, Elvira

    2017-01-01

    In the present work, tracing and Whatman papers were used as substrates to grow zinc oxide (ZnO) nanostructures. Cellulose-based substrates are cost-efficient, highly sensitive and environmentally friendly. ZnO nanostructures with hexagonal structure were synthesized by hydrothermal under microwave irradiation using an ultrafast approach, that is, a fixed synthesis time of 10 min. The effect of synthesis temperature on ZnO nanostructures was investigated from 70 to 130 °C. An Ultra Violet (UV)/Ozone treatment directly to the ZnO seed layer prior to microwave assisted synthesis revealed expressive differences regarding formation of the ZnO nanostructures. Structural characterization of the microwave synthesized materials was carried out by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The optical characterization has also been performed. The time resolved photocurrent of the devices in response to the UV turn on/off was investigated and it has been observed that the ZnO nanorod arrays grown on Whatman paper substrate present a responsivity 3 times superior than the ones grown on tracing paper. By using ZnO nanorods, the surface area-to-volume ratio will increase and will improve the sensor sensibility, making these types of materials good candidates for low cost and disposable UV sensors. The sensors were exposed to bending tests, proving their high stability, flexibility and adaptability to different surfaces. PMID:29140304

  1. Determination of trace elements of Egyptian cane sugar (Naga Hammady factories) by neutron activation, atomic absorption spectrophotometric and inductively coupled plasma-atomic emission spectrometric analyses.

    PubMed

    Awadallah, R M; Sherif, M K; Mohamed, A E; Grass, F

    1984-01-01

    INAA, AAS and ICP-AES techniques are applied to the determination of trace amounts of Ag, Al, As, Au, Ba, Br, Ca, Cd, Ce, Cl, Co, Cr, Cs, Cu, Dy, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in the stalks of sugar cane plant after extracting juice, raw juice principal (mixed) juice, juice withdrawn from the successive stages of sugar industry, sirup, deposits from evaporators, molasse, A-? and B-sugar and in the soil samples (collected from the field supplying the factories by cane plants) taken from the immediate vicinity of the plant roots at surface, 30 and 60 cm depth. The results obtained are in a good agreement of the safety baselines of using juice as beverage, molasse derivatives (honey, sweets, ...) as diet for common people in the developed countries and in industry (methanol, ethanol, acetone & acetic acid, ...) and sugar sweeting for many purposes (in beverages, desserts, ...). Differences of trace elements concentrations in soil samples may be reasoned to geochemical and biogeochemical fractionation while those in juice may be due to the changes in the environmental conditions, chemical composition and botanic structures. Variations in trace element contents in the products formed during the successive stages of sugar industry may be a result of evaporation, filtration processes, chemical treatments or corrosion of vessels, containers or engines. Trace elements are very important where they are responsible for enzymatic and biochemical reactions, matabolism, health and diseases.

  2. Ultra-Performance Liquid Chromatographic Determination of Tocopherols and Retinol in Human Plasma

    PubMed Central

    Bell, Edward C.; John, Mathew; Hughes, Rodney J.; Pham, Thu

    2014-01-01

    A rapid, selective and sensitive ultra-performance liquid chromatography method has been developed for the detection and quantification of tocopherols and retinol in human plasma. Alpha-tocopherol, gamma-tocopherol and retinol are assayed using fluorescence detection. Excitation/emission wavelengths are 295/330 nm and 325/470 nm for the analysis of both tocopherols and retinol, respectively. Retinol acetate is employed as the internal standard. The reversed-phase method incorporates gradient elution with a mobile phase consisting of methanol and acetonitrile. Separation of vitamin compounds is achieved using a bridged ethyl hybrid C18 column. The retention times for retinol, retinol acetate, gamma-tocopherol and alpha-tocopherol are 1.6, 1.8, 3.9 and 4.3 min, respectively. The limits of quantification for retinol, gamma-tocopherol and alpha-tocopherol were 0.02, 0.02 and 0.1 µg/mL, respectively. The assay method is suitable for the analysis of tocopherols and retinol in human plasma. The method may be applied following the ingestion of foods fortified with these fat-soluble vitamins. PMID:24170122

  3. Detection and Monitoring of Toxic Chemical at Ultra Trace Level by Utilizing Doped Nanomaterial

    PubMed Central

    Khan, Sher Bahadar; Rahman, Mohammed M.; Akhtar, Kalsoom; Asiri, Abdullah M.

    2014-01-01

    Composite nanoparticles were synthesized by eco-friendly hydrothermal process and characterized by different spectroscopic techniques. All the spectroscopic techniques suggested the synthesis of well crystalline optically active composite nanoparticles with average diameter of ∼30 nm. The synthesized nanoparticles were applied for the development of chemical sensor which was fabricated by coating the nanoparticles on silver electrode for the recognition of phthalimide using simple I–V technique. The developed sensor exhibited high sensitivity (1.7361 µA.mM−1.cm−2), lower detection limit (8.0 µM) and long range of detection (77.0 µM to 0.38 M). Further the resistances of composite nanoparticles based sensor was found to be 2.7 MΩ which change from 2.7 to 1.7 with change in phthalimide concentration. The major advantages of the designed sensor over existing sensors are its simple technique, low cost, lower detection limit, high sensitivity and long range of detection. It can detect phthalimide even at trace level and sense over wide range of concentrations. Therefore the composite nanoparticals would be a better choice for the fabrication of phthalimide chemical sensor and would be time and cost substituted implement for environmental safety. PMID:25329666

  4. Dodecylbenzene sulfonate-coated magnetite nanoparticles as a new adsorbent for solid phase extraction-spectrophotometric determination of ultra trace amounts of ammonium in water samples.

    PubMed

    Eskandari, Habibollah; Shariati, Mohammad Reza

    2011-10-17

    A new method was proposed for the determination of ammonium based on the preconcentration with dodecylbenzene sulfonate modified magnetite nanoparticles. Ammonium was oxidized to nitrite by hypobromite and then the nitrite produced was determined spectrophotometrically, using sulfabenzamide and N-(1-naphthyl) ethylenediamine after solid phase extraction. The azo dye produced was desorbed by an appropriate small volume of sodium hydroxide prior to the absorbance measurement. The linear calibration graphs were obtained in the concentration range of 0.03-6.00 ng mL(-1) ammonium. The relative standard deviation and recovery percents were 1.0 and 99.0, respectively, for 1.0 ng mL(-1) ammonium, and the limit of detection was 3.2 ng L(-1) ammonium. The interfering effects of a large number of diverse ions on the determination of ammonium were studied. The method was applied to the determination of ammonium in various types of water resources. The results revealed a high efficiency for the recommended ammonium determination method. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Developing a Trace Element Biosignature for Early Earth and Mars

    NASA Astrophysics Data System (ADS)

    Gangidine, A.; Czaja, A. D.; Havig, J.

    2018-04-01

    Due to metamorphism and diagenesis, determining the biogenicity of ancient fossils is difficult and often contentious. Using trace element concentrations, we propose a novel biosignature independent from organic and morphological preservation.

  6. Miniaturized hollow fibre assisted liquid-phase microextraction and gas chromatography for determination of trace concentration of sufentanil and alfentanil in biological samples.

    PubMed

    Fakhari, Ali Reza; Tabani, Hadi; Nojavan, Saeed

    2013-07-01

    A simple and highly sensitive method that involves miniaturized hollow fibre assisted liquid-phase microextraction with gas chromatography-flame ionization detector was developed for the determination of trace concentration of sufentanil and alfentanil in biological samples. These drugs were extracted from 5 ml of aqueous solution with pH 10.0 into an organic extracting solvent (1-octanol) impregnated in the pores and lumen of a hollow fibre. After extraction for a prescribed time, 2.0 µl of the extraction solvent was injected directly in to the GC injection port. Under the optimized conditions, (1-octanol as extracting solvent, stirring rate of 700 rpm, 15% (w/v) salt addition, pH 10.0 and 25 min sampling time at 50 °C) large enrichment factors of 535 and 420 were achieved for sufentanil and alfentanil, respectively. Dynamic linear ranges were in the range of 0.05 to 500 ng/ml for sufentanil and 0.1 to 500 ng/ml for alfentanil. Limits of detection 0.01 and 0.02 ng/ml were obtained for sufentanil and alfentanil, respectively. The percent relative intra-day and inter-day standard deviations were found to be less than 8.4% (n = 5). Finally, this method was successfully applied for the separation, preconcentration and determination of trace concentration of sufentanil and alfentanil in plasma and urine samples. Copyright © 2012 John Wiley & Sons, Ltd.

  7. Ultra-low dose naltrexone enhances cannabinoid-induced antinociception.

    PubMed

    Paquette, Jay; Olmstead, Mary C; Olmstead, Mary

    2005-12-01

    Both opioids and cannabinoids have inhibitory effects at micromolar doses, which are mediated by activated receptors coupling to Gi/o-proteins. Surprisingly, the analgesic effects of opioids are enhanced by ultra-low doses (nanomolar to picomolar) of the opioid antagonist, naltrexone. As opioid and cannabinoid systems interact, this study investigated whether ultra-low dose naltrexone also influences cannabinoid-induced antinociception. Separate groups of Long-Evans rats were tested for antinociception following an injection of vehicle, a sub-maximal dose of the cannabinoid agonist WIN 55 212-2, naltrexone (an ultra-low or a high dose) or a combination of WIN 55 212-2 and naltrexone doses. Tail-flick latencies were recorded for 3 h, at 10-min intervals for the first hour, and at 15-min intervals thereafter. Ultra-low dose naltrexone elevated WIN 55 212-2-induced tail flick thresholds without extending its duration of action. This enhancement was replicated in animals receiving intraperitoneal or intravenous injections. A high dose of naltrexone had no effect on WIN 55 212-2-induced tail flick latencies, but a high dose of the cannabinoid 1 receptor antagonist SR 141716 blocked the elevated tail-flick thresholds produced by WIN 55 212-2+ultra-low dose naltrexone. These data suggest a mechanism of cannabinoid-opioid interaction whereby activated opioid receptors that couple to Gs-proteins may attenuate cannabinoid-induced antinociception and/or motor functioning.

  8. The Low-Mass Stellar Initial Mass Function: Ultra-Faint Dwarf Galaxies Revisited

    NASA Astrophysics Data System (ADS)

    Platais, Imants

    2017-08-01

    The stellar Initial Mass Function plays a critical role in the evolution of the baryonic content of the Universe. The form of the low-mass IMF - stars of mass less than the solar mass - determines the fraction of baryons locked up for a Hubble time, and thus indicates how gas and metals are cycled through galaxies. Inferences from resolved stellar populations, where the low-mass luminosity function and associated IMF can be derived from direct star counts, generally favor an invariant and universal IMF. However, a recent study of ultra-faint dwarf galaxies Hercules and Leo IV indicates a bottom-lite IMF, over a narrow range of stellar mass (only 0.55-0.75 M_sun), correlated with the internal velocity dispersion and/or metallicity. We propose to obtain ultra-deep imaging for a significantly closer ultra-faint dwarf, Bootes I, which will allow us to construct the luminosity function down to M_v=+10 (equivalent to 0.35 solar mass). We will also re-analyze the HST archival observations for the Hercules and Leo IV dwarfs using the same updated techniques as for Bootes I. The combined datasets should provide a reliable answer to the question of how variable is the low-mass stellar IMF.

  9. Determination of the chemical properties of residues retained in individual cloud droplets by XRF microprobe at SPring-8

    NASA Astrophysics Data System (ADS)

    Ma, C.-J.; Tohno, S.; Kasahara, M.; Hayakawa, S.

    2004-06-01

    To determine the chemical properties of residue retained in individual cloud droplets is primarily important for the understanding of rainout mechanism and aerosol modification in droplet. The sampling of individual cloud droplets were carried out on the summit of Mt. Taiko located in Tango peninsula, Kyoto prefecture, during Asian dust storm event in March of 2002. XRF microprobe system equipped at SPring-8, BL-37XU was applied to the subsequent quantification analysis of ultra trace elements in residues of individual cloud droplets. It was possible to form the replicas of separated individual cloud droplets on the thin collodion film. The two dimensional XRF maps for the residues in individual cloud droplets were clearly drawn by scanning of micro-beam. Also, XRF spectra of trace elements in residues were well resolved. From the XRF spectra for individual residues, the chemical mixed state of residues could be assumed. The chemical forms of Fe (Fe +++) and Zn (Zn +) could be clearly characterized by their K-edge micro-XANES spectra. By comparison of Z/Si mass ratios of residues in cloud droplets and those of the original sands collected in desert areas in China, the aging of ambient dust particles and their in cloud modification were indirectly assumed.

  10. Determination of Trace Level Triclosan in Water by Online Preconcentration and HPLC-UV Diode Array

    EPA Science Inventory

    An online high performance liquid chromatography (HPLC) method for the detection and quantification of trace levels of triclosan in water is discussed. Triclosan, an anti-bacterial agent, and related compounds have been shown to reach municipal waste waters through the disposal ...

  11. Trace element geochemistry of Archean volcanic rocks

    NASA Technical Reports Server (NTRS)

    Jahn, B.-M.; Shih, C.-Y.; Murthy, V. R.

    1974-01-01

    The K, Rb, Sr, Ba and rare-earth-element contents of some Archean volcanic rocks from the Vermilion greenstone belt, northeast Minnesota, were determined by the isotopic dilution method. The characteristics of trace element abundances, supported by the field occurrences and major element chemistry, suggest that these volcanic rocks were formed in an ancient island arc system.

  12. Validation of a method for simultaneous determination of nitroimidazoles, benzimidazoles and chloramphenicols in swine tissues by ultra-high performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Xia, Xi; Wang, Yuanyuan; Wang, Xia; Li, Yun; Zhong, Feng; Li, Xiaowei; Huang, Yaoling; Ding, Shuangyang; Shen, Jianzhong

    2013-05-31

    This paper presents a sensitive and confirmatory multi-residue method for the analysis of 23 veterinary drugs and metabolites belonging to three classes (nitroimidazoles, benzimidazoles, and chloramphenicols) in porcine muscle, liver, and kidney. After extracted with ethyl acetate and basic ethyl acetate sequentially, the crude extracts were defatted with hexane and further purified using Oasis MCX solid-phase extraction cartridges. Rapid determination was carried out by ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Data acquisition was performed under positive and negative mode simultaneously. Recoveries based on matrix-matched calibrations for meat, liver, and kidney ranged from 50.6 to 108.1%. The method quantification limits were in the range of 3-100ng/kg. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Characterization of Polyimide Foams for Ultra-Lightweight Space Structures

    NASA Technical Reports Server (NTRS)

    Meador, Michael (Technical Monitor); Hillman, Keithan; Veazie, David R.

    2003-01-01

    Ultra-lightweight materials have played a significant role in nearly every area of human activity ranging from magnetic tapes and artificial organs to atmospheric balloons and space inflatables. The application range of ultra-lightweight materials in past decades has expanded dramatically due to their unsurpassed efficiency in terms of low weight and high compliance properties. A new generation of ultra-lightweight materials involving advanced polymeric materials, such as TEEK (TM) polyimide foams, is beginning to emerge to produce novel performance from ultra-lightweight systems for space applications. As a result, they require that special conditions be fulfilled to ensure adequate structural performance, shape retention, and thermal stability. It is therefore important and essential to develop methodologies for predicting the complex properties of ultra-lightweight foams. To support NASA programs such as the Reusable Launch Vehicle (RLV), Clark Atlanta University, along with SORDAL, Inc., has initiated projects for commercial process development of polyimide foams for the proposed cryogenic tank integrated structure (see figure 1). Fabrication and characterization of high temperature, advanced aerospace-grade polyimide foams and filled foam sandwich composites for specified lifetimes in NASA space applications, as well as quantifying the lifetime of components, are immensely attractive goals. In order to improve the development, durability, safety, and life cycle performance of ultra-lightweight polymeric foams, test methods for the properties are constant concerns in terms of timeliness, reliability, and cost. A major challenge is to identify the mechanisms of failures (i.e., core failure, interfacial debonding, and crack development) that are reflected in the measured properties. The long-term goal of the this research is to develop the tools and capabilities necessary to successfully engineer ultra-lightweight polymeric foams. The desire is to reduce density

  14. Generation of a large volume of clinically relevant nanometre-sized ultra-high-molecular-weight polyethylene wear particles for cell culture studies

    PubMed Central

    Ingham, Eileen; Fisher, John; Tipper, Joanne L

    2014-01-01

    It has recently been shown that the wear of ultra-high-molecular-weight polyethylene in hip and knee prostheses leads to the generation of nanometre-sized particles, in addition to micron-sized particles. The biological activity of nanometre-sized ultra-high-molecular-weight polyethylene wear particles has not, however, previously been studied due to difficulties in generating sufficient volumes of nanometre-sized ultra-high-molecular-weight polyethylene wear particles suitable for cell culture studies. In this study, wear simulation methods were investigated to generate a large volume of endotoxin-free clinically relevant nanometre-sized ultra-high-molecular-weight polyethylene wear particles. Both single-station and six-station multidirectional pin-on-plate wear simulators were used to generate ultra-high-molecular-weight polyethylene wear particles under sterile and non-sterile conditions. Microbial contamination and endotoxin levels in the lubricants were determined. The results indicated that microbial contamination was absent and endotoxin levels were low and within acceptable limits for the pharmaceutical industry, when a six-station pin-on-plate wear simulator was used to generate ultra-high-molecular-weight polyethylene wear particles in a non-sterile environment. Different pore-sized polycarbonate filters were investigated to isolate nanometre-sized ultra-high-molecular-weight polyethylene wear particles from the wear test lubricants. The use of the filter sequence of 10, 1, 0.1, 0.1 and 0.015 µm pore sizes allowed successful isolation of ultra-high-molecular-weight polyethylene wear particles with a size range of < 100 nm, which was suitable for cell culture studies. PMID:24658586

  15. Generation of a large volume of clinically relevant nanometre-sized ultra-high-molecular-weight polyethylene wear particles for cell culture studies.

    PubMed

    Liu, Aiqin; Ingham, Eileen; Fisher, John; Tipper, Joanne L

    2014-04-01

    It has recently been shown that the wear of ultra-high-molecular-weight polyethylene in hip and knee prostheses leads to the generation of nanometre-sized particles, in addition to micron-sized particles. The biological activity of nanometre-sized ultra-high-molecular-weight polyethylene wear particles has not, however, previously been studied due to difficulties in generating sufficient volumes of nanometre-sized ultra-high-molecular-weight polyethylene wear particles suitable for cell culture studies. In this study, wear simulation methods were investigated to generate a large volume of endotoxin-free clinically relevant nanometre-sized ultra-high-molecular-weight polyethylene wear particles. Both single-station and six-station multidirectional pin-on-plate wear simulators were used to generate ultra-high-molecular-weight polyethylene wear particles under sterile and non-sterile conditions. Microbial contamination and endotoxin levels in the lubricants were determined. The results indicated that microbial contamination was absent and endotoxin levels were low and within acceptable limits for the pharmaceutical industry, when a six-station pin-on-plate wear simulator was used to generate ultra-high-molecular-weight polyethylene wear particles in a non-sterile environment. Different pore-sized polycarbonate filters were investigated to isolate nanometre-sized ultra-high-molecular-weight polyethylene wear particles from the wear test lubricants. The use of the filter sequence of 10, 1, 0.1, 0.1 and 0.015 µm pore sizes allowed successful isolation of ultra-high-molecular-weight polyethylene wear particles with a size range of < 100 nm, which was suitable for cell culture studies.

  16. Rubidium-traced white-light etalon calibrator for radial velocity measurements at the cm s-1 level

    NASA Astrophysics Data System (ADS)

    Stürmer, Julian; Seifahrt, Andreas; Schwab, Christian; Bean, Jacob L.

    2017-04-01

    We report on the construction and testing of a vacuum-gap Fabry-Pérot etalon calibrator for high precision radial velocity spectrographs. Our etalon is traced against a rubidium frequency standard to provide a cost effective, yet ultra precise wavelength reference. We describe here a turn-key system working at 500 to 900 nm, ready to be installed at any current and next-generation radial velocity spectrograph that requires calibration over a wide spectral bandpass. Where appropriate, we have used off-the-shelf, commercial components with demonstrated long-term performance to accelerate the development timescale of this instrument. Our system combines for the first time the advantages of passively stabilized etalons for optical and near-infrared wavelengths with the laser-locking technique demonstrated for single-mode fiber etalons. We realize uncertainties in the position of one etalon line at the 10 cm s-1 level in individual measurements taken at 4 Hz. When binning the data over 10 s, we are able to trace the etalon line with a precision of better than 3 cm s-1. We present data obtained during a week of continuous operation where we detect (and correct for) the predicted, but previously unobserved shrinking of the etalon Zerodur spacer corresponding to a shift of 13 cm s-1 per day.

  17. Ultra-processed foods and the nutritional dietary profile in Brazil

    PubMed Central

    Louzada, Maria Laura da Costa; Martins, Ana Paula Bortoletto; Canella, Daniela Silva; Baraldi, Larissa Galastri; Levy, Renata Bertazzi; Claro, Rafael Moreira; Moubarac, Jean-Claude; Cannon, Geoffrey; Monteiro, Carlos Augusto

    2015-01-01

    OBJECTIVE To assess the impact of consuming ultra-processed foods on the nutritional dietary profile in Brazil. METHODS Cross-sectional study conducted with data from the module on individual food consumption from the 2008-2009 Pesquisa de Orçamentos Familiares (POF – Brazilian Family Budgets Survey). The sample, which represented the section of the Brazilian population aged 10 years or over, involved 32,898 individuals. Food consumption was evaluated by two 24-hour food records. The consumed food items were classified into three groups: natural or minimally processed, including culinary preparations with these foods used as a base; processed; and ultra-processed. RESULTS The average daily energy consumption per capita was 1,866 kcal, with 69.5% being provided by natural or minimally processed foods, 9.0% by processed foods and 21.5% by ultra-processed food. The nutritional profile of the fraction of ultra-processed food consumption showed higher energy density, higher overall fat content, higher saturated and trans fat, higher levels of free sugar and less fiber, protein, sodium and potassium, when compared to the fraction of consumption related to natural or minimally processed foods. Ultra-processed foods presented generally unfavorable characteristics when compared to processed foods. Greater inclusion of ultra-processed foods in the diet resulted in a general deterioration in the dietary nutritional profile. The indicators of the nutritional dietary profile of Brazilians who consumed less ultra-processed foods, with the exception of sodium, are the stratum of the population closer to international recommendations for a healthy diet. CONCLUSIONS The results from this study highlight the damage to health that is arising based on the observed trend in Brazil of replacing traditional meals, based on natural or minimally processed foods, with ultra-processed foods. These results also support the recommendation of avoiding the consumption of these kinds of foods

  18. Ultra-processed foods and the nutritional dietary profile in Brazil.

    PubMed

    Costa Louzada, Maria Laura da; Martins, Ana Paula Bortoletto; Canella, Daniela Silva; Baraldi, Larissa Galastri; Levy, Renata Bertazzi; Claro, Rafael Moreira; Moubarac, Jean-Claude; Cannon, Geoffrey; Monteiro, Carlos Augusto

    2015-01-01

    OBJECTIVE To assess the impact of consuming ultra-processed foods on the nutritional dietary profile in Brazil. METHODS Cross-sectional study conducted with data from the module on individual food consumption from the 2008-2009 Pesquisa de Orçamentos Familiares (POF - Brazilian Family Budgets Survey). The sample, which represented the section of the Brazilian population aged 10 years or over, involved 32,898 individuals. Food consumption was evaluated by two 24-hour food records. The consumed food items were classified into three groups: natural or minimally processed, including culinary preparations with these foods used as a base; processed; and ultra-processed. RESULTS The average daily energy consumption per capita was 1,866 kcal, with 69.5% being provided by natural or minimally processed foods, 9.0% by processed foods and 21.5% by ultra-processed food. The nutritional profile of the fraction of ultra-processed food consumption showed higher energy density, higher overall fat content, higher saturated and trans fat, higher levels of free sugar and less fiber, protein, sodium and potassium, when compared to the fraction of consumption related to natural or minimally processed foods. Ultra-processed foods presented generally unfavorable characteristics when compared to processed foods. Greater inclusion of ultra-processed foods in the diet resulted in a general deterioration in the dietary nutritional profile. The indicators of the nutritional dietary profile of Brazilians who consumed less ultra-processed foods, with the exception of sodium, are the stratum of the population closer to international recommendations for a healthy diet. CONCLUSIONS The results from this study highlight the damage to health that is arising based on the observed trend in Brazil of replacing traditional meals, based on natural or minimally processed foods, with ultra-processed foods. These results also support the recommendation of avoiding the consumption of these kinds of foods.

  19. UltraSail CubeSat Solar Sail Flight Experiment

    NASA Technical Reports Server (NTRS)

    Carroll, David; Burton, Rodney; Coverstone, Victoria; Swenson, Gary

    2013-01-01

    UltraSail is a next-generation, highrisk, high-payoff sail system for the launch, deployment, stabilization, and control of very large (km2 class) solar sails enabling high payload mass fractions for interplanetary and deep space spacecraft. UltraSail is a non-traditional approach to propulsion technology achieved by combining propulsion and control systems developed for formation- flying microsatellites with an innovative solar sail architecture to achieve controllable sail areas approaching 1 km2, sail subsystem area densities approaching 1 g/m2, and thrust levels many times those of ion thrusters used for comparable deep space missions. UltraSail can achieve outer planetary rendezvous, a deep-space capability now reserved for high-mass nuclear and chemical systems. There is a twofold rationale behind the UltraSail concept for advanced solar sail systems. The first is that sail-andboom systems are inherently size-limited. The boom mass must be kept small, and column buckling limits the boom length to a few hundred meters. By eliminating the boom, UltraSail not only offers larger sail area, but also lower areal density, allowing larger payloads and shorter mission transit times. The second rationale for UltraSail is that sail films present deployment handling difficulties as the film thickness approaches one micrometer. The square sail requires that the film be folded in two directions for launch, and similarly unfolded for deployment. The film is stressed at the intersection of two folds, and this stress varies inversely with the film thickness. This stress can cause the film to yield, forming a permanent crease, or worse, to perforate. By rolling the film as UltraSail does, creases are prevented. Because the film is so thin, the roll thickness is small. Dynamic structural analysis of UltraSail coupled with dynamic control analysis shows that the system can be designed to eliminate longitudinal torsional waves created while controlling the pitch of the blades

  20. The role of sample preparation in interpretation of trace element concentration variability in moss bioindication studies

    USGS Publications Warehouse

    Migaszewski, Z.M.; Lamothe, P.J.; Crock, J.G.; Galuszka, A.; Dolegowska, S.

    2011-01-01

    Trace element concentrations in plant bioindicators are often determined to assess the quality of the environment. Instrumental methods used for trace element determination require digestion of samples. There are different methods of sample preparation for trace element analysis, and the selection of the best method should be fitted for the purpose of a study. Our hypothesis is that the method of sample preparation is important for interpretation of the results. Here we compare the results of 36 element determinations performed by ICP-MS on ashed and on acid-digested (HNO3, H2O2) samples of two moss species (Hylocomium splendens and Pleurozium schreberi) collected in Alaska and in south-central Poland. We found that dry ashing of the moss samples prior to analysis resulted in considerably lower detection limits of all the elements examined. We also show that this sample preparation technique facilitated the determination of interregional and interspecies differences in the chemistry of trace elements. Compared to the Polish mosses, the Alaskan mosses displayed more positive correlations of the major rock-forming elements with ash content, reflecting those elements' geogenic origin. Of the two moss species, P. schreberi from both Alaska and Poland was also highlighted by a larger number of positive element pair correlations. The cluster analysis suggests that the more uniform element distribution pattern of the Polish mosses primarily reflects regional air pollution sources. Our study has shown that the method of sample preparation is an important factor in statistical interpretation of the results of trace element determinations. ?? 2010 Springer-Verlag.

  1. Determination of major elements by wavelength-dispersive X-ray fluorescence spectrometry and trace elements by inductively coupled plasma mass spectrometry in igneous rocks from the same fused sample (110 mg)

    NASA Astrophysics Data System (ADS)

    Amosova, Alena A.; Panteeva, Svetlana V.; Chubarov, Victor M.; Finkelshtein, Alexandr L.

    2016-08-01

    The fusion technique is proposed for simultaneous determination of 35 elements from the same sample. Only 110 mg of rock sample was used to obtain fused glasses for quantitative determination of 10 major elements by wavelength dispersive X-ray fluorescence analysis, 16 rare earth elements and some other trace elements by inductively coupled plasma mass spectrometry analysis. Fusion was performed with 1.1 g of lithium metaborate and LiBr solution as the releasing agent in platinum crucible in electric furnace at 1100 °C. The certified reference materials of ultramafic, mafic, intermediate and felsic igneous rocks have been applied to obtain the calibration curves for rock-forming oxides (Na2O, MgO, Al2O3, SiO2, P2O5, K2O, CaO, TiO2, MnO, Fe2O3) and some trace elements (Ba, Sr, Zr) determination by X-ray fluorescence analysis. The repeatability does not exceed the allowable standard deviation for a wide range of concentrations. In the most cases the relative standard deviation was less than 5%. Obtained glasses were utilized for the further determination of rare earth (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) and some other (Ba, Sr, Zr, Rb, Cs, Y, Nb, Hf, Ta, Th and U) trace elements by inductively coupled plasma mass spectrometry analysis with the same certified reference materials employed. The results could mostly be accepted as satisfactory. The proposed procedure essentially reduces the expenses in comparison with separate sample preparation for inductively coupled plasma mass spectrometry and X-ray fluorescence analysis.

  2. Trace elements in dialysis.

    PubMed

    Filler, Guido; Felder, Sarah

    2014-08-01

    In end-stage chronic kidney disease (CKD), pediatric nephrologists must consider the homeostasis of the multiple water-soluble ions that are influenced by renal replacement therapy (RRT). While certain ions such as potassium and calcium are closely monitored, little is known about the handling of trace elements in pediatric dialysis. RRT may lead to accumulation of toxic trace elements, either due to insufficient elimination or due to contamination, or to excessive removal of essential trace elements. However, trace elements are not routinely monitored in dialysis patients and no mechanism for these deficits or toxicities has been established. This review summarizes the handling of trace elements, with particular attention to pediatric data. The best data describe lead and indicate that there is a higher prevalence of elevated lead (Pb, atomic number 82) levels in children on RRT when compared to adults. Lead is particularly toxic in neurodevelopment and lead levels should therefore be monitored. Monitoring of zinc (Zn, atomic number 30) and selenium (Se, atomic number 34) may be indicated in the monitoring of all pediatric dialysis patients to reduce morbidity from deficiency. Prospective studies evaluating the impact of abnormal trace elements and the possible therapeutic value of intervention are required.

  3. Brain MR imaging at ultra-low radiofrequency power.

    PubMed

    Sarkar, Subhendra N; Alsop, David C; Madhuranthakam, Ananth J; Busse, Reed F; Robson, Philip M; Rofsky, Neil M; Hackney, David B

    2011-05-01

    To explore the lower limits for radiofrequency (RF) power-induced specific absorption rate (SAR) achievable at 1.5 T for brain magnetic resonance (MR) imaging without loss of tissue signal or contrast present in high-SAR clinical imaging in order to create a potentially viable MR method at ultra-low RF power to image tissues containing implanted devices. An institutional review board-approved HIPAA-compliant prospective MR study design was used, with written informed consent from all subjects prior to MR sessions. Seven healthy subjects were imaged prospectively at 1.5 T with ultra-low-SAR optimized three-dimensional (3D) fast spin-echo (FSE) and fluid-attenuated inversion-recovery (FLAIR) T2-weighted sequences and an ultra-low-SAR 3D spoiled gradient-recalled acquisition in the steady state T1-weighted sequence. Corresponding high-SAR two-dimensional (2D) clinical sequences were also performed. In addition to qualitative comparisons, absolute signal-to-noise ratios (SNRs) and contrast-to-noise ratios (CNRs) for multicoil, parallel imaging acquisitions were generated by using a Monte Carlo method for quantitative comparison between ultra-low-SAR and high-SAR results. There were minor to moderate differences in the absolute tissue SNR and CNR values and in qualitative appearance of brain images obtained by using ultra-low-SAR and high-SAR techniques. High-SAR 2D T2-weighted imaging produced slightly higher SNR, while ultra-low-SAR 3D technique not only produced higher SNR for T1-weighted and FLAIR images but also higher CNRs for all three sequences for most of the brain tissues. The 3D techniques adopted here led to a decrease in the absorbed RF power by two orders of magnitude at 1.5 T, and still the image quality was preserved within clinically acceptable imaging times. RSNA, 2011

  4. HMM based automated wheelchair navigation using EOG traces in EEG

    NASA Astrophysics Data System (ADS)

    Aziz, Fayeem; Arof, Hamzah; Mokhtar, Norrima; Mubin, Marizan

    2014-10-01

    This paper presents a wheelchair navigation system based on a hidden Markov model (HMM), which we developed to assist those with restricted mobility. The semi-autonomous system is equipped with obstacle/collision avoidance sensors and it takes the electrooculography (EOG) signal traces from the user as commands to maneuver the wheelchair. The EOG traces originate from eyeball and eyelid movements and they are embedded in EEG signals collected from the scalp of the user at three different locations. Features extracted from the EOG traces are used to determine whether the eyes are open or closed, and whether the eyes are gazing to the right, center, or left. These features are utilized as inputs to a few support vector machine (SVM) classifiers, whose outputs are regarded as observations to an HMM. The HMM determines the state of the system and generates commands for navigating the wheelchair accordingly. The use of simple features and the implementation of a sliding window that captures important signatures in the EOG traces result in a fast execution time and high classification rates. The wheelchair is equipped with a proximity sensor and it can move forward and backward in three directions. The asynchronous system achieved an average classification rate of 98% when tested with online data while its average execution time was less than 1 s. It was also tested in a navigation experiment where all of the participants managed to complete the tasks successfully without collisions.

  5. HMM based automated wheelchair navigation using EOG traces in EEG.

    PubMed

    Aziz, Fayeem; Arof, Hamzah; Mokhtar, Norrima; Mubin, Marizan

    2014-10-01

    This paper presents a wheelchair navigation system based on a hidden Markov model (HMM), which we developed to assist those with restricted mobility. The semi-autonomous system is equipped with obstacle/collision avoidance sensors and it takes the electrooculography (EOG) signal traces from the user as commands to maneuver the wheelchair. The EOG traces originate from eyeball and eyelid movements and they are embedded in EEG signals collected from the scalp of the user at three different locations. Features extracted from the EOG traces are used to determine whether the eyes are open or closed, and whether the eyes are gazing to the right, center, or left. These features are utilized as inputs to a few support vector machine (SVM) classifiers, whose outputs are regarded as observations to an HMM. The HMM determines the state of the system and generates commands for navigating the wheelchair accordingly. The use of simple features and the implementation of a sliding window that captures important signatures in the EOG traces result in a fast execution time and high classification rates. The wheelchair is equipped with a proximity sensor and it can move forward and backward in three directions. The asynchronous system achieved an average classification rate of 98% when tested with online data while its average execution time was less than 1 s. It was also tested in a navigation experiment where all of the participants managed to complete the tasks successfully without collisions.

  6. Water and sodium intake habits and status of ultra-endurance runners during a multi-stage ultra-marathon conducted in a hot ambient environment: an observational field based study

    PubMed Central

    2013-01-01

    Background Anecdotal evidence suggests ultra-runners may not be consuming sufficient water through foods and fluids to maintenance euhydration, and present sub-optimal sodium intakes, throughout multi-stage ultra-marathon (MSUM) competitions in the heat. Subsequently, the aims were primarily to assess water and sodium intake habits of recreational ultra-runners during a five stage 225 km semi self-sufficient MSUM conducted in a hot ambient environment (Tmax range: 32°C to 40°C); simultaneously to monitor serum sodium concentration, and hydration status using multiple hydration assessment techniques. Methods Total daily, pre-stage, during running, and post-stage water and sodium ingestion of ultra-endurance runners (UER, n = 74) and control (CON, n = 12) through foods and fluids were recorded on Stages 1 to 4 by trained dietetic researchers using dietary recall interview technique, and analysed through dietary analysis software. Body mass (BM), hydration status, and serum sodium concentration were determined pre- and post-Stages 1 to 5. Results Water (overall mean (SD): total daily 7.7 (1.5) L/day, during running 732 (183) ml/h) and sodium (total daily 3.9 (1.3) g/day, during running 270 (151) mg/L) ingestion did not differ between stages in UER (p < 0.001 vs. CON). Exercise-induced BM loss was 2.4 (1.2)% (p < 0.001). Pre- to post-stage BM gains were observed in 26% of UER along competition. Pre- and post-stage plasma osmolality remained within normal clinical reference range (280 to 303 mOsmol/kg) in the majority of UER (p > 0.05 vs. CON pre-stage). Asymptomatic hyponatraemia (<135 mmol/L) was evident pre- and post-stage in n = 8 UER, corresponding to 42% of sampled participants. Pre- and post-stage urine colour, urine osmolality and urine/plasma osmolality ratio increased (p < 0.001) as competition progressed in UER, with no change in CON. Plasma volume and extra-cellular water increased (p < 0.001) 22.8% and 9.2%, respectively

  7. Ultra-wide-field imaging in diabetic retinopathy.

    PubMed

    Ghasemi Falavarjani, Khalil; Tsui, Irena; Sadda, Srinivas R

    2017-10-01

    Since 1991, 7-field images captured with 30-50 degree cameras in the Early Treatment Diabetic Retinopathy Study were the gold standard for fundus imaging to study diabetic retinopathy. Ultra-wide-field images cover significantly more area (up to 82%) of the fundus and with ocular steering can in many cases image 100% of the fundus ("panretinal"). Recent advances in image analysis of ultra-wide-field imaging allow for precise measurements of the peripheral retinal lesions. There is a growing consensus in the literature that ultra-wide-field imaging improves detection of peripheral lesions in diabetic retinopathy and leads to more accurate classification of the disease. There is discordance among studies, however, on the correlation between peripheral diabetic lesions and diabetic macular edema and optimal management strategies to treat diabetic retinopathy. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Methodology for processing pressure traces used as inputs for combustion analyses in diesel engines

    NASA Astrophysics Data System (ADS)

    Rašić, Davor; Vihar, Rok; Žvar Baškovič, Urban; Katrašnik, Tomaž

    2017-05-01

    This study proposes a novel methodology for designing an optimum equiripple finite impulse response (FIR) filter for processing in-cylinder pressure traces of a diesel internal combustion engine, which serve as inputs for high-precision combustion analyses. The proposed automated workflow is based on an innovative approach of determining the transition band frequencies and optimum filter order. The methodology is based on discrete Fourier transform analysis, which is the first step to estimate the location of the pass-band and stop-band frequencies. The second step uses short-time Fourier transform analysis to refine the estimated aforementioned frequencies. These pass-band and stop-band frequencies are further used to determine the most appropriate FIR filter order. The most widely used existing methods for estimating the FIR filter order are not effective in suppressing the oscillations in the rate- of-heat-release (ROHR) trace, thus hindering the accuracy of combustion analyses. To address this problem, an innovative method for determining the order of an FIR filter is proposed in this study. This method is based on the minimization of the integral of normalized signal-to-noise differences between the stop-band frequency and the Nyquist frequency. Developed filters were validated using spectral analysis and calculation of the ROHR. The validation results showed that the filters designed using the proposed innovative method were superior compared with those using the existing methods for all analyzed cases. Highlights • Pressure traces of a diesel engine were processed by finite impulse response (FIR) filters with different orders • Transition band frequencies were determined with an innovative method based on discrete Fourier transform and short-time Fourier transform • Spectral analyses showed deficiencies of existing methods in determining the FIR filter order • A new method of determining the FIR filter order for processing pressure traces was

  9. Trace elements and their distribution in protein fractions of camel milk in comparison to other commonly consumed milks.

    PubMed

    Al-Awadi, F M; Srikumar, T S

    2001-08-01

    Studies on camels' milk, whether with respect to concentration or bioavailability of trace elements from this milk, are limited and warrant further investigation. The object of this study was to analyse the concentration and distribution of zinc, copper, selenium, manganese and iron in camel milk compared to those in human milk, cows' milk and infant formula under similar experimental conditions. Camels' milk and cows' milk were collected from local farms, human milk samples were obtained from healthy donors in Kuwait and infant formula was purchased locally. Milk fractionation was performed by ultra-centrifugation and gelcolumn chromatography. The concentration of trace elements was analysed by atomic absorption spectrometry and that of protein was determined spectrophotometrically. The concentration of manganese and iron in camels' milk was remarkably higher (7-20-fold and 4-10-fold, respectively) than in human milk, cows' milk and infant formula. The zinc content of camels' milk was higher than that of human milk but slightly lower than in cows' milk and infant formula. The concentration of copper in camels' milk was similar to that of cows' milk but lower than in human milk and infant formula. The selenium content of camels' milk was comparable to those of other types of milk, Approximately 50-80% of zinc, copper and manganese in camels' milk were associated with the casein fraction, similar to that of cows' milk, The majority of selenium and iron in camels' milk was in association with the low molecular weight fraction, It is recommended that camels' milk be considered as a potential source of manganese, selenium and iron, perhaps not only for infants, but also for other groups suspected of mild deficiency of these elements. Further investigations are required to confirm this proposal.

  10. Determination of the proton-to-helium ratio in cosmic rays at ultra-high energies from the tail of the Xmax distribution

    NASA Astrophysics Data System (ADS)

    Yushkov, A.; Risse, M.; Werner, M.; Krieg, J.

    2016-12-01

    We present a method to determine the proton-to-helium ratio in cosmic rays at ultra-high energies. It makes use of the exponential slope, Λ, of the tail of the Xmax distribution measured by an air shower experiment. The method is quite robust with respect to uncertainties from modeling hadronic interactions and to systematic errors on Xmax and energy, and to the possible presence of primary nuclei heavier than helium. Obtaining the proton-to-helium ratio with air shower experiments would be a remarkable achievement. To quantify the applicability of a particular mass-sensitive variable for mass composition analysis despite hadronic uncertainties we introduce as a metric the 'analysis indicator' and find an improved performance of the Λ method compared to other variables currently used in the literature. The fraction of events in the tail of the Xmax distribution can provide additional information on the presence of nuclei heavier than helium in the primary beam.

  11. Boninite-like intraplate magmas from Manihiki Plateau require ultra-depleted and enriched source components

    PubMed Central

    Golowin, Roman; Portnyagin, Maxim; Hoernle, Kaj; Hauff, Folkmar; Gurenko, Andrey; Garbe-Schönberg, Dieter; Werner, Reinhard; Turner, Simon

    2017-01-01

    The Ontong Java and Manihiki oceanic plateaus are believed to have formed through high-degree melting of a mantle plume head. Boninite-like, low-Ti basement rocks at Manihiki, however, imply a more complex magma genesis compared with Ontong Java basement lavas that can be generated by ∼30% melting of a primitive mantle source. Here we show that the trace element and isotope compositions of low-Ti Manihiki rocks can best be explained by re-melting of an ultra-depleted source (possibly a common mantle component in the Ontong Java and Manihiki plume sources) re-enriched by ≤1% of an ocean-island-basalt-like melt component. Unlike boninites formed via hydrous flux melting of refractory mantle at subduction zones, these boninite-like intraplate rocks formed through adiabatic decompression melting of refractory plume material that has been metasomatized by ocean-island-basalt-like melts. Our results suggest that caution is required before assuming all Archaean boninites were formed in association with subduction processes. PMID:28181497

  12. Rapid determination of yunaconitine and related alkaloids in aconites and aconite-containing drugs by ultra high-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Song, Long; Zhang, Hong; Liu, Xin; Zhao, Zhi-Li; Chen, Shi-Lin; Wang, Zheng-Tao; Xu, Hong-Xi

    2012-12-01

    Yunaconitine (YAC) is a toxic aconite alkaloid that is considered to be a hidden aconite poison since it is frequently found in body fluids from aconite poisoning patients, but has not been well studied in commonly used herbal drugs. In this paper, a rapid and sensitive ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) detection combined with microwave-assisted extraction (MAE) was developed for high throughput simultaneous determination of YAC and six other toxic aconite alkaloids in 31 samples of crude, processed aconites and aconite-containing drugs. The optimized method showed excellent linearity, precision, accuracy and recovery for all target compounds with short run time. YAC was detected in some samples with contents from 0.015 to 10.41 mg/g. This is the first report on the determination of YAC in Radix Aconiti, Radix Aconiti Kusnezoffii and aconite-containing drugs. This newly developed method facilitates the rapid screening of YAC and related toxic aconite alkaloids and allows YAC to be used as a chemical marker for the quality control of aconites and aconite-containing drugs. Copyright © 2012 John Wiley & Sons, Ltd.

  13. Ultra-high Temperature Emittance Measurements for Space and Missile Applications

    NASA Technical Reports Server (NTRS)

    Rogers, Jan; Crandall, David

    2009-01-01

    Advanced modeling and design efforts for many aerospace components require high temperature emittance data. Applications requiring emittance data include propulsion systems, radiators, aeroshells, heatshields/thermal protection systems, and leading edge surfaces. The objective of this work is to provide emittance data at ultra-high temperatures. MSFC has a new instrument for the measurement of emittance at ultra-high temperatures, the Ultra-High Temperature Emissometer System (Ultra-HITEMS). AZ Technology Inc. developed the instrument, designed to provide emittance measurements over the temperature range 700-3500K. The Ultra-HITEMS instrument measures the emittance of samples, heated by lasers, in vacuum, using a blackbody source and a Fourier Transform Spectrometer. Detectors in a Nicolet 6700 FT-IR spectrometer measure emittance over the spectral range of 0.4-25 microns. Emitted energy from the specimen and output from a Mikron M390S blackbody source at the same temperature with matched collection geometry are measured. Integrating emittance over the spectral range yields the total emittance. The ratio provides a direct measure of total hemispherical emittance. Samples are heated using lasers. Optical pyrometry provides temperature data. Optical filters prevent interference from the heating lasers. Data for Inconel 718 show excellent agreement with results from literature and ASTM 835. Measurements taken from levitated spherical specimens provide total hemispherical emittance data; measurements taken from flat specimens mounted in the chamber provide near-normal emittance data. Data from selected characterization studies will be presented. The Ultra-HITEMS technique could advance space and missile technologies by advancing the knowledge base and the technology readiness level for ultra-high temperature materials.

  14. Influence of trace elements on dental enamel properties: A review.

    PubMed

    Qamar, Zeeshan; Haji Abdul Rahim, Zubaidah Binti; Chew, Hooi Pin; Fatima, Tayyaba

    2017-01-01

    Dental enamel, an avascular, irreparable, outermost and protective layer of the human clinical crown has a potential to withstand the physico-chemical effects and forces. These properties are being regulated by a unique association among elements occurring in the crystallites setup of human dental enamel. Calcium and phosphate are the major components (hydroxyapatite) in addition to some trace elements which have a profound effect on enamel. The current review was planned to determine the aptitude of various trace elements to substitute and their influence on human dental enamel in terms of physical and chemical properties.

  15. Ultra-low noise supercontinuum source for ultra-high resolution optical coherence tomography at 1300 nm

    NASA Astrophysics Data System (ADS)

    Gonzalo, I. B.; Maria, M.; Engelsholm, R. D.; Feuchter, T.; Leick, L.; Moselund, P. M.; Podoleanu, A.; Bang, O.

    2018-02-01

    Supercontinuum (SC) sources are of great interest for many applications due to their ultra-broad optical bandwidth, good beam quality and high power spectral density [1]. In particular, the high average power over large bandwidths makes SC light sources excellent candidates for ultra-high resolution optical coherence tomography (UHR-OCT) [2-5]. However, conventional SC sources suffer from high pulse-to-pulse intensity fluctuations as a result of the noise-sensitive nonlinear effects involved in the SC generation process [6-9]. This intensity noise from the SC source can limit the performance of OCT, resulting in a reduced signal-to-noise ratio (SNR) [10-12]. Much work has been done to reduce the noise of the SC sources for instance with fiber tapers [7,8] or increasing the repetition rate of the pump laser for averaging in the spectrometer [10,12]. An alternative approach is to use all-normal dispersion (ANDi) fibers [13,14] to generate SC light from well-known coherent nonlinear processes [15-17]. In fact, reduction of SC noise using ANDi fibers compared to anomalous dispersion SC pumped by sub-picosecond pulses has been recently demonstrated [18], but a cladding mode was used to stabilize the ANDi SC. In this work, we characterize the noise performance of a femtosecond pumped ANDi based SC and a commercial SC source in an UHR-OCT system at 1300 nm. We show that the ANDi based SC presents exceptional noise properties compared to a commercial source. An improvement of 5 dB in SNR is measured in the UHR-OCT system, and the noise behavior resembles that of a superluminiscent diode. This preliminary study is a step forward towards development of an ultra-low noise SC source at 1300 nm for ultra-high resolution OCT.

  16. Solar University-National Lab Ultra-Effective Program | Photovoltaic

    Science.gov Websites

    Lab Ultra-Effective Program Solar University-National lab Ultra-effective Program (SUN UP) was created scientists arise out of long-standing collaborations. SUN UP was created to facilitate these interactions of a young man working in a laboratory setting with equipment. The goal of SUN UP is to increase the

  17. Ultra-fast switching of light by absorption saturation in vacuum ultra-violet region.

    PubMed

    Yoneda, Hitoki; Inubushi, Yuichi; Tanaka, Toshihiro; Yamaguchi, Yuta; Sato, Fumiya; Morimoto, Shunsuke; Kumagai, Taisuke; Nagasono, Mitsuru; Higashiya, Atsushi; Yabashi, Makina; Ishikawa, Tetsuya; Ohashi, Haruhiko; Kimura, Hiroaki; Kitamura, Hikaru; Kodama, Ryosuke

    2009-12-21

    Advances in free electron lasers producing high energy photons [Nat. Photonics 2(9), 555-559 (2008)] are expected to open up a new science of nonlinear optics of high energy photons. Specifically, lasers of photon energy higher than the plasma frequency of a metal can show new interaction features because they can penetrate deeply into metals without strong reflection. Here we show the observation of ultra-fast switching of vacuum ultra-violet (VUV) light caused by saturable absorption of a solid metal target. A strong gating is observed at energy fluences above 6J/cm2 at wavelength of 51 nm with tin metal thin layers. The ratio of the transmission at high intensity to low intensity is typically greater than 100:1. This means we can design new nonlinear photonic devices such as auto-correlator and pulse slicer for the VUV region.

  18. Added sugars and ultra-processed foods in Spanish households (1990-2010).

    PubMed

    Latasa, P; Louzada, M L D C; Martinez Steele, E; Monteiro, C A

    2017-12-26

    To study the association between ultra-processed foods acquisitions and added sugar content of total food purchases in Spanish households in 2010. Changes over time (1990-2000-2010) in ultra-processed food purchases and added sugars content of total food purchases are also compared. We used data from three nationally representative Household Budget Surveys (HBS) conducted in 1990, 2000 and 2010. Number of studied households was 21,012, 33,730 and 22,116, respectively. Purchased foods and drinks were classified according to NOVA food groups as ultra-processed foods, processed foods, unprocessed or minimally processed foods, or processed culinary ingredients. Linear and Poisson regressions were used to estimate the association between quintiles of energy contribution of ultra-processed foods and added sugars contents of total food purchases in 2010. Changes over time were assessed using tests of linear trend and Student's t test. In 2010, ultra-processed foods represented 31.7% of daily energy acquisitions and 80.4% of all added sugars. Added sugars content of food purchases raised from 7.3% in the lowest to 18.2% in the highest quintiles of energy contribution of ultra-processed foods. The risk of exceeding 10% energy from added sugars quadrupled between the lowest and highest quintiles. The percentage of ultra-processed foods on all food purchases almost tripled between 1990 and 2010 (from 11.0 to 31.7%), paralleling the increase of added sugars content (from 8.4 to 13.0%). Cutting down exceeding added sugars availability in Spain may require a reduction in ultra-processed food purchasing.

  19. Determination and fingerprint analysis of steroidal saponins in roots of Liriope muscari (Decne.) L. H. Bailey by ultra high performance liquid chromatography coupled with ion trap time-of-flight mass spectrometry.

    PubMed

    Li, Yong-Wei; Qi, Jin; Wen-Zhang; Zhou, Shui-Ping; Yan-Wu; Yu, Bo-Yang

    2014-07-01

    Liriope muscari (Decne.) L. H. Bailey is a well-known traditional Chinese medicine used for treating cough and insomnia. There are few reports on the quality evaluation of this herb partly because the major steroid saponins are not readily identified by UV detectors and are not easily isolated due to the existence of many similar isomers. In this study, a qualitative and quantitative method was developed to analyze the major components in L. muscari (Decne.) L. H. Bailey roots. Sixteen components were deduced and identified primarily by the information obtained from ultra high performance liquid chromatography with ion-trap time-of-flight mass spectrometry. The method demonstrated the desired specificity, linearity, stability, precision, and accuracy for simultaneous determination of 15 constituents (13 steroidal glycosides, 25(R)-ruscogenin, and pentylbenzoate) in 26 samples from different origins. The fingerprint was established, and the evaluation was achieved using similarity analysis and principal component analysis of 15 fingerprint peaks from 26 samples by ultra high performance liquid chromatography. The results from similarity analysis were consistent with those of principal component analysis. All results suggest that the established method could be applied effectively to the determination of multi-ingredients and fingerprint analysis of steroid saponins for quality assessment and control of L. muscari (Decne.) L. H. Bailey. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. PIXE analysis of caries related trace elements in tooth enamel

    NASA Astrophysics Data System (ADS)

    Annegarn, H. J.; Jodaikin, A.; Cleaton-Jones, P. E.; Sellschop, J. P. F.; Madiba, C. C. P.; Bibby, D.

    1981-03-01

    PIXE analysis has been applied to a set of twenty human teeth to determine trace element concentration in enamel from areas susceptible to dental caries (mesial and distal contact points) and in areas less susceptible to the disease (buccal surfaces), with the aim of determining the possible roles of trace elements in the curious process. The samples were caries-free anterior incisors extracted for periodontal reasons from subjects 10-30 years of age. Prior to extraction of the sample teeth, a detailed dental history and examination was carried out in each individual. PIXE analysis, using a 3 MeV proton beam of 1 mm diameter, allowed the determination of Ca, Mn, Fe, Cu, Zn, Sr and Pb above detection limits. As demonstrated in this work, the enhanced sensitivity of PIXE analysis over electron microprobe analysis, and the capability of localised surface analysis compared with the pooled samples required for neutron activation analysis, makes it a powerful and useful technique in dental analysis.