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Sample records for absorption spectrometric detection

  1. Nasal absorption studies of granisetron in rats using a validated high-performance liquid chromatographic method with mass spectrometric detection.

    Science.gov (United States)

    Woo, Jong Soo

    2007-06-01

    Granisetron is a selective 5-HT3 receptor antagonist that is used therapeutically for the prevention of vomiting and nausea associated with emetogenic cancer chemotherapy. Although forms of the drug are commercially available for intravenous and oral dosage, there is a need for intranasal delivery formulations in specific patient populations in which the use of these dosage forms may be unfeasible and/or inconvenient. A rapid and specific high-performance liq uid chromatography method with mass spectrometric detection (LC-MS) was developed and validated for the analysis of granisetron in plasma after nasal administration in rats. Granisetron was separated in a reverse-phase C-18 column without interference from other components of plasma. This method involves a rapid assay for the determination of granisetron in a small volume of plasma with a run time of 12 min using ondansetron as an internal standard. Data were acquired in the electrospray ionization (ESI) mode with positive ion detection and application of single ion recording (SIR). Granisetron and ondansetron were detected at m/z values of 313.2 and 294.2, respectively. The method described was found to be suitable for the analysis of all samples collected during preclinical pharmacokinetic investigations of granisetron in rats after nasal administration. To date, the first pharmacokinetic study after intranasal administration of granisetron was performed and some pharmacokinetic parameters were presented in this paper. Granisetron was found to be well absorbed through nasal route and the bioavailability of this drug following nasal administration was comparable with that of intravenous administration. PMID:17679558

  2. Inclusion of riboflavin in β-cyclodextrin: A fluorimetric and absorption spectrometric study

    Science.gov (United States)

    Roy, Dalim Kumar; Deb, Nipamanjari; Ghosh, Bankim Chandra; Mukherjee, Asok K.

    2009-07-01

    Formation of inclusion complexes between riboflavin and β-cyclodextrin (β-CD) with both 1:1 and 1:2 stoichiometry has been established by fluorimetric titration. However, in absorption spectrometric experiment, spectral change of riboflavin in the visible range could be observed only by taking β-CD at a much higher concentration (about 100 times) than riboflavin and under such condition only 1:2 complexes could be detected. Its formation constant ( K) was determined by a multiple linear regression analysis of the absorption data. The reliability of the K value was confirmed by the consistency achieved on analyzing the data at two different wavelengths.

  3. Spectrofluorimetric, Atomic Absorption Spectrometric and Spectrophotometric Determination of Some Fluoroquinolones

    Directory of Open Access Journals (Sweden)

    Hesham Salem

    2005-01-01

    Full Text Available Simple, accurate, sensitive and selective spectrofluorimetric, atomic absorption spectrometric and spectrophotometric methods are described for the quantitative determination of ten fluoroquinolones (amifloxacin, ciprofloxacin hydrochloride, difloxacin hydrochloride, enoxacin, enrofloxacin, lomefloxacin hydrochloride, levofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate. The first method was a spectrofluorimetric method in which samples of the studied drugs in 0.1 N H2SO4 showed native fluorescence at 450 nm when excitation was at 290 nm. The calibration graph was rectilinear from 0.3-1.4 μg mL-1 (method I. Cobalt sulphate was used for precipitation of the ion associates formed from the reaction with the cited drugs. The formation and solubility of the solid complexes at the optimum conditions of pH and ionic strength values have been studied. The method depends on direct determination of the ions in the precipitate or indirect determination of the ions in the filtrate by atomic absorption spectroscopy. The optimum conditions for precipitation were carefully studied. Rectilinear calibration graphs were obtained in the range of 3-30 μg mL-1 for each of the investigated drugs. The molar ratios of the formed chelats were determined by Job's method and their association constants were also calculated (method II. Ammonium vanadate was used for the spectrophotometric determination of the selected fluoroquinolones by oxidation in sulphuric acid medium resulting in the development of a greenish blue colour measured at 766 nm which was attributed to the vanadium (IV produced by reduction of vanadium (V by the selected drugs. The optimum conditions for heating time, reagent concentration and sulphuric acid concentration were carefully studied. The accuracy and precision of the proposed method was confirmed by estimating five or six replicates within Beer's law limits were obtained in the range 10-40 μg mL-1 for each of the investigated drugs

  4. Graphite furnace atomic absorption spectrometric detection of vanadium in water and food samples after solid phase extraction on multiwalled carbon nanotubes.

    Science.gov (United States)

    Wadhwa, Sham Kumar; Tuzen, Mustafa; Gul Kazi, Tasneem; Soylak, Mustafa

    2013-11-15

    Vanadium(V) ions as 8-hydroxyquinoline chelates were loaded on multiwalled carbon nanotubes (MWNTs) in a mini chromatographic column. Vanadium was determined by graphite furnace atomic absorption spectrometry (GFAAS). Various analytical parameters including pH of the working solutions, amounts of 8-hydroxyquinoline, eluent type, sample volume, and flow rates were investigated. The effects of matrix ions and some transition metals were also studied. The column can be reused 250 times without any loss in its sorption properties. The preconcentration factor was found as 100. Detection limit (3 s) and limit of quantification (10 s) for the vanadium in the optimal conditions were observed to be 0.012 µg L(-1) and 0.040 μg L(-1), respectively. The capacity of adsorption was 9.6 mg g(-1). Relative standard deviation (RSD) was found to be 5%. The validation of the method was confirmed by using NIST SRM 1515 Apple leaves, NIST SRM 1570a Spinach leaves and GBW 07605 Tea certified reference materials. The procedure was applied to the determination of vanadium in tap water and bottled drinking water samples. The procedure was also successfully applied to microwave digested food samples including black tea, coffee, tomato, cabbage, zucchini, apple and chicken samples.

  5. Generation of volatile copper species after in situ ionic liquid formation dispersive liquid-liquid microextraction prior to atomic absorption spectrometric detection.

    Science.gov (United States)

    Stanisz, Ewa; Zgoła-Grześkowiak, Agnieszka; Matusiewicz, Henryk

    2014-11-01

    The new procedure using in situ synthesis of ionic liquid extractant for dispersive liquid-liquid microextraction (in situ IL DLLME) combined with generation of volatile species prior to electrothermal atomic absorption spectrometry (ET AAS) for the determination of copper in soil samples was developed. Analytical signals were obtained without the back-extraction of copper from the IL phase prior to its determination. Under optimal conditions, the extraction in 10 mL of sample solution employing 8 μL of 1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (HmimNTf2) (as the extraction solvent) was conducted. The ionic liquid served as two-task reagent: the efficient extractant and enhancement substance for generation step. The chemical generation of volatile species was performed by reduction of acidified copper solution (HCl 0.8 mol L(-1)) with NaBH4 (1.5%). Some essential parameters of the chemical generation such as NaBH4 and HCl concentrations, the kind and concentration of ionic liquid, carrier gas (Ar) flow rate, reaction and trapping time as well as pyrolysis and atomization temperatures were studied. For photogeneration the effect of the parameters such as the kind and concentration of low molecular weight organic acids and ionic liquid, carrier gas (Ar) flow rate, UV irradiation and ultrasonication time on the analytical signals were studied. The detection limit was found as 1.8 ng mL(-1) and the relative standard deviation (RSD) for seven replicate measurements of 100 µg mL(-1) in sample solution was 7%. The accuracy of the proposed method was evaluated by analysis of the certified reference materials. The measured copper contents in the reference materials were in satisfactory agreement with the certified values. The method was successfully applied to analysis of the soil and sediment samples. PMID:25127592

  6. Automated sequential injection-microcolumn approach with on-line flame atomic absorption spectrometric detection for implementing metal fractionation schemes of homogeneous and non-homogeneous solid samples of environmental interest

    DEFF Research Database (Denmark)

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald;

    2005-01-01

    spectrometric detection and used for the determination of Cu as a model analyte, the potentials of this novel hyphenated approach are demonstrated by the ability of handling up to 300 mg sample of a nonhomogeneous sewage amended soil (viz., CRM 483). The three steps of the endorsed Standards, Measurements...

  7. Atomic absorption spectrometric determination of mineral elements in mammalian bones

    International Nuclear Information System (INIS)

    The phosphorus content of the major bones of male and female selected mammals was determined using the yellow vanadomolybdate colorimetric method. For each animal, the bone with the highest phosphorus content was used as pilot sample. Varying concentrations of strontium were added to solutions of the ashed pilot samples to minimize phosphorus interference in the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 6,000 ppm (0.6%) of strontium was required to give optimum results for calcium. The amount of magnesium obtained from the analysis was not affected by the addition of strontium. With the incorporation of strontium in the sample solution, all elements of interest can be determined in the same sample solution. Based on this, a procedure is proposed for the determination of calcium and other elements in bones. Average recoveries of spiked calcium and magnesium were 97.85% and 98.16%, respectively at the 95% confidence level. The coefficients of variation obtained for replicate determinations using one of the samples were 0.00% for calcium, lead and sodium, 2.93% for magnesium, 3.27% for iron and 3.92% for zinc at the concentration levels found in that sample. Results from the proposed procedure compared well with those from classical chemical methods at the 95% confidence level. It is evident that calcium phosphorus, magnesium and sodium which are the most abundant elements in the bones are distributed in varying amounts both in the different types of bones and different animal species, although the general trend is Ca > P > Na > Mg for each bone considered. The calcium - phosphorus ratio is generally 3:1. The work set out to propose an atomic absorption spectrometric method for the multi-element analysis of mammalian bones with a single sample preparation and to study the distribution pattern of these elements in the bones. (Author)

  8. The determination of trace amounts of heavy metals in waters by a flow-injection system including ion-exchange preconcentration and flame atomic absorption spectrometric detection

    International Nuclear Information System (INIS)

    The flow-injection system combines on-line ion-exchange preconcentration with atomic absorption spectrometry (a.a.s.) for the determination of traces (μg l-1) of heavy metals in water samples. A multifunctional rotary sampling valve which incorporated two parallel sampling columns allows sampling, exchange, elution and a.a.s. to be achieved sequentially. The increases in sensitivity for nickel, copper, lead and cadmium were 20-28-fold at a sampling rate of 40 h-1 with 5-ml samples. Relative standard deviations were 1.5-4.1%. The recoveries of these four metals added to tap, sea and polluted waters were generally satisfactory, except for cadmium in polluted water. The effects of column diameter and elution flow rates on sensitivity are discussed. Possible interferences are described. (Auth.)

  9. Optimization of the preconcentration system of cadmium with 1(2-thiazolylazo)-p-cresol using a knotted reactor and flame atomic absorption spectrometric detection

    International Nuclear Information System (INIS)

    The present paper proposes an on-line preconcentration procedure for cadmium determination in drinking water samples. It is based on the precipitation of cadmium(II) ions on a knotted reactor (KR) using 1(2-thiazolylazo)-p-cresol (TAC) as complexing reagent. The optimization step was performed using a full factorial design involving the variables: pH, eluent concentration (nitric acid) and TAC concentration. The results of this experiment demonstrated that these variables at chosen levels are not statistically significant. Under optimized experimental established conditions, analytical parameters for the preconcentration method were: a detection limit of 40.0 ng/l, precision as relative standard deviation (RSD) of 1.2 and 1.0%, for cadmium concentration of 2.5 and 20.0 μg/l, respectively. The preconcentration factor considering the slopes of the analytical curves with and without preconcentration is 23 for a sample volume of 10 ml. This system shows a sampling frequency of 25 h-1. In order to check the accuracy, the standard reference material, NIST SRM 1643d trace elements in water was analyzed. A comparison, using t-test demonstrates that there is not significant difference among the achieved results with proposed method and the certified values. The addition/recovery experiments in the samples analyzed demonstrated the accuracy and applicability of the system developed for cadmium determination in water samples

  10. Mass spectrometric detection, identification, and fragmentation of arseno-phytochelatins.

    Science.gov (United States)

    Schmied-Tobies, Maria I H; Arroyo-Abad, Uriel; Mattusch, Jürgen; Reemtsma, Thorsten

    2014-11-01

    Phytochelatins (PC) are cystein-rich oligopeptides in plants for coordination with toxic metals and metalloids via their thiol groups. The composition, structure, and mass spectrometric fragmentation of arseno-PC (As-PC) with PC of different degree of oligomerization (PC2-PC5) in solution were studied using liquid chromatography coupled in parallel to inductively coupled plasma mass spectrometry and electrospray ionization quadrupole time-of-flight mass spectrometry. As-PC were detected from As(PC2) to As(PC5) with an increasing number of isomers that differ in the position of thiol groups bound to As. Thermodynamic modeling supported the identification process in case of these isomers. Mass spectrometric fragmentation of the As-PC does not follow the established pattern of peptides but is governed by the formation of series of As-containing annular cations, which coordinate to As via S, N, or O. Structure proposals for 30 As-PC fragment ions in the range m/z 147.92 to m/z 1290.18 are elaborated. Many of these fragment ions are characteristic to several As-PC and may be suited for a screening for As-PC in plant extracts. The mass spectrometric data offer the perspective for a future more sensitive determination of As-PC by means of liquid chromatography tandem mass spectrometry with multiple reaction monitoring. PMID:25395130

  11. Mass spectrometric detection, identification, and fragmentation of arseno-phytochelatins.

    Science.gov (United States)

    Schmied-Tobies, Maria I H; Arroyo-Abad, Uriel; Mattusch, Jürgen; Reemtsma, Thorsten

    2014-11-01

    Phytochelatins (PC) are cystein-rich oligopeptides in plants for coordination with toxic metals and metalloids via their thiol groups. The composition, structure, and mass spectrometric fragmentation of arseno-PC (As-PC) with PC of different degree of oligomerization (PC2-PC5) in solution were studied using liquid chromatography coupled in parallel to inductively coupled plasma mass spectrometry and electrospray ionization quadrupole time-of-flight mass spectrometry. As-PC were detected from As(PC2) to As(PC5) with an increasing number of isomers that differ in the position of thiol groups bound to As. Thermodynamic modeling supported the identification process in case of these isomers. Mass spectrometric fragmentation of the As-PC does not follow the established pattern of peptides but is governed by the formation of series of As-containing annular cations, which coordinate to As via S, N, or O. Structure proposals for 30 As-PC fragment ions in the range m/z 147.92 to m/z 1290.18 are elaborated. Many of these fragment ions are characteristic to several As-PC and may be suited for a screening for As-PC in plant extracts. The mass spectrometric data offer the perspective for a future more sensitive determination of As-PC by means of liquid chromatography tandem mass spectrometry with multiple reaction monitoring.

  12. Novel atomic absorption spectrometric and rapid spectrophotometric methods for the quantitation of paracetamol in saliva: Application to pharmacokinetic studies

    Directory of Open Access Journals (Sweden)

    Issa M

    2008-01-01

    Full Text Available A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III (method I; oxidation of p-aminophenol after the hydrolysis of paracetamol (method II. Iron (II then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 µg/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 µg/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 µg/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%.

  13. Electrothermal atomization atomic absorption spectrometric determination of trace metals in uranium-plutomium fuel materials

    International Nuclear Information System (INIS)

    Atomic absorption spectrometric methods using the electrothermal mode of atomization developed for the determination of Ag, Be, Ca, Cd, Cr, Co, Cu, Fe, Li, Mn, Na, Ni, Sn and Zn in (U, Pu) solution with 4% plutonium have been described. The carbon rod atomizer has been adapted for glove box operation to enable handling of plutonium containing solution samples. Multielement solution standards with graded concentrations of the analytes and fixed concentration of the matrix are used in the standardization process. Nanogram to sub-nanogram quantities of the analytes have been determined with a precision of better than 9% RSD using 5 μl of the sample aliquots. (orig.)

  14. Status of mass spectrometric radiocarbon detection at ETHZ

    Science.gov (United States)

    Seiler, Martin; Maxeiner, Sascha; Wacker, Lukas; Synal, Hans-Arno

    2015-10-01

    A prototype of a mass spectrometric radiocarbon detection instrument without accelerator stage was built for the first time and set into operation at ETH Zurich. The system is designed as an experimental platform to optimize performance of 14C detection at low ion energies and to study the most relevant processes that may limit system performance. The optimized stripper unit incorporates differential pumping to maintain a low gas outflow and a revised tube design to better match the phase space volume of the ion beam at low energies. The system is fully operational and has demonstrated true radiocarbon dating capabilities. The overall beam transmission through the stripper tube is about 40% for the 1+ charge state. Radiocarbon analyses with an overall precision of 0.6% were obtained on a single sample under regular measurement conditions. By analyzing multiple targets of the same sample material an uncertainty level of 0.3% has been reached. The background level corresponds to a radiocarbon age of 40,000 years.

  15. Colorimetric and atomic absorption spectrometric determination of mucolytic drug ambroxol through ion-pair formation with iron and thiocyanate.

    Science.gov (United States)

    Levent, Abdulkadir; Sentürk, Zühre

    2010-09-01

    Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection.

  16. Separation of trace antimony and arsenic prior to hydride generation atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    A separation method utilizing a synthetic zeolite (mordenite) was developed in order to eliminate the gas phase interference of Sb(III) on As(III) during quartz furnace hydride generation atomic absorption spectrometric (HGAAS) determination. The efficiency of the proposed separation method in the reduction of suppression effects of transition metal ions on As(III) signal was also investigated. Among the volatile hydride-forming elements and their different oxidation states tested (Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), and Te(VI)), only Sb(III) was found to have a signal depression effect even at low (μg l-1) concentrations under the experimental conditions employed. It has been shown that mordenite adsorbs Sb(III) quantitatively, even at a concentration of 1000 μg l-1, at pHs greater than two, and also, it reduces the initial concentrations of the transition metal ions to lower levels which can be tolerated in many studies. The adsorption of Sb(III) on mordenite follows the Freundlich isotherm and is endothermic in nature

  17. Mass spectrometric detection of radiocarbon for dating applications

    Energy Technology Data Exchange (ETDEWEB)

    Synal, H.-A., E-mail: synal@phys.ethz.ch [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland); Schulze-Koenig, T.; Seiler, M.; Suter, M.; Wacker, L. [ETH Zurich, Laboratory of Ion Beam Physics, Building HPK, 8093 Zurich (Switzerland)

    2013-01-15

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV {sup 14}C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  18. Mass spectrometric detection of radiocarbon for dating applications

    Science.gov (United States)

    Synal, H.-A.; Schulze-König, T.; Seiler, M.; Suter, M.; Wacker, L.

    2013-01-01

    Radiocarbon is still the most important nuclide measured by accelerator mass spectrometry (AMS). The related capabilities for dating and tracer studies are eminent not only in archaeology but also drive important applications in the earth and environmental sciences as well as in biomedical research. So far, standard mass spectrometric systems have not been capable of radiocarbon dating because of interfering molecular isobars which, however, can be completely eliminated in charge changing processes at high ion beam energies (MeV) [1,2]. Here, we present a novel type mass spectrometry system for radiocarbon analyses. Radiocarbon dating was performed using 45 keV 14C ions from the ion source and a molecule dissociation unit kept at ground potential. This proof-of-principle experiment demonstrates for the first time the feasibility of mass spectrometric radiocarbon dating without an accelerator. The results obtained will be the basis of an optimized design for a radiocarbon dating instrument comparable in size, complexity and cost to standard mass spectrometers.

  19. Atomic-absorption spectrometric determination of trace metals in zirconium and zircaloy by discrete sample nebulization

    International Nuclear Information System (INIS)

    A discrete sample nebulization technique was employed to determine trace metals in nuclear grade zirconium and Zircaloy by flame atomic-absorption spectrometry. With 10% (w/v) sample solutions, detection limits for Cd, Cu, Mn, Ni and Pb were 0.6, 2, 1, 3, and 10 μg/g. Micro standard-addition procedures and background correction were employed to minimize matrix interferences produced by the high salt content of the aspirated solutions. (author)

  20. Quantification of salsolinol enantiomers by stable isotope dilution liquid chromatography with tandem mass spectrometric detection

    OpenAIRE

    Cai, Min; Liu, Yi-Ming

    2008-01-01

    Salsolinol, 1-methyl-6,7-dihydroxy-2,3,4,5-tetrahydroisoquinoline (SAL), is a precursor of a Parkinsonian neurotoxin, N-methysalsolinol (N-methyl-SAL). Previous studies have shown that individual enantiomers of N-methyl-SAL possess distinct neurotoxicological properties. In this work, a chiral high-performance liquid chromatography (HPLC) method with electrospray ionization tandem mass spectrometric (ESI-MS/MS) detection was developed for the quantification of (R/S)-SAL enantiomers. Enantiose...

  1. Mass Spectrometric Detection of Nanoparticle Host–Guest Interactions in Cells

    OpenAIRE

    Yan, Bo; Yesilbag Tonga, Gulen; Hou, Singyuk; Fedick, Patrick W.; Yeh, Yi-Cheun; Alfonso, Felix S.; Mizuhara, Tsukasa; Vachet, Richard W.; Rotello, Vincent M.

    2014-01-01

    Synthetic host–guest chemistry is a versatile tool for biomedical applications. Characterization and detection of host–guest complexes in biological systems, however, is challenging due to the complexity of the biological milieu. Here, we describe and apply a mass spectrometric method to monitor the association and dissociation of nanoparticle (NP)-based host–guest interactions that integrates NP-assisted laser desorption/ionization (LDI) and matrix assisted laser desoption/ionization (MALDI)...

  2. Mass spectrometric approaches to detecting prions and protein conformers

    Science.gov (United States)

    Transmissible spongiform encephalopathies (TSEs) can cause substantial economic damage to agriculture. These diseases have characteristically long incubation periods, comparatively short symptomatic intervals, and are invariably fatal. Early detection is important in controlling these diseases. Howe...

  3. Novel absorption detection techniques for capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Xue, Y.

    1994-07-27

    Capillary electrophoresis (CE) has emerged as one of the most versatile separation methods. However, efficient separation is not sufficient unless coupled to adequate detection. The narrow inner diameter (I.D.) of the capillary column raises a big challenge to detection methods. For UV-vis absorption detection, the concentration sensitivity is only at the {mu}M level. Most commercial CE instruments are equipped with incoherent UV-vis lamps. Low-brightness, instability and inefficient coupling of the light source with the capillary limit the further improvement of UV-vis absorption detection in CE. The goals of this research have been to show the utility of laser-based absorption detection. The approaches involve: on-column double-beam laser absorption detection and its application to the detection of small ions and proteins, and absorption detection with the bubble-shaped flow cell.

  4. Experimental determination of the self-absorption factor for MTR plates by passive gamma spectrometric measurement

    Science.gov (United States)

    Berndt, R.; Mortreau, P.

    2011-07-01

    The measurement of the absolute activity or the mass of radioactive substances by gamma spectrometry needs to include a correction for the radiation absorption inside the source volume, the so-called self-absorption factor. It depends on geometry and material composition of the source, the detector geometry and on the geometrical arrangement of source and gamma radiation detector; it can be calculated if full information about all that is available. This article however describes how to determine the self-absorption factor from measurements if the radiation sources are plates of uranium fuel with typical parameters of nuclear fuel for MTR reactors and without using detail information on the source geometry, thus allowing easy inspection without relying on - potentially falsified - declarations on the internal properties of the fuel objects and without calculation.

  5. Experimental determination of the self-absorption factor for MTR plates by passive gamma spectrometric measurement

    Energy Technology Data Exchange (ETDEWEB)

    Berndt, R., E-mail: Reinhard.Berndt@jrc.ec.europa.eu [European Commission, Joint Research Centre, Institute for Transuranium Elements, TP 800, Via Fermi, Ispra (Italy); Mortreau, P. [European Commission, Joint Research Centre, Institute for Transuranium Elements, TP 800, Via Fermi, Ispra (Italy)

    2011-07-11

    The measurement of the absolute activity or the mass of radioactive substances by gamma spectrometry needs to include a correction for the radiation absorption inside the source volume, the so-called self-absorption factor. It depends on geometry and material composition of the source, the detector geometry and on the geometrical arrangement of source and gamma radiation detector; it can be calculated if full information about all that is available. This article however describes how to determine the self-absorption factor from measurements if the radiation sources are plates of uranium fuel with typical parameters of nuclear fuel for MTR reactors and without using detail information on the source geometry, thus allowing easy inspection without relying on - potentially falsified - declarations on the internal properties of the fuel objects and without calculation.

  6. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    International Nuclear Information System (INIS)

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation (n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits (k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l-1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples

  7. Flame atomic absorption spectrometric determination of cadmium(II) and lead(II) after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493

    International Nuclear Information System (INIS)

    An enrichment procedure for cadmium and lead after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493 has been established prior to their flame atomic absorption spectrometric determinations. The analytical parameters including pH, amounts of dibenzyldithiocarbamate, sample volume, etc., were investigated. The effects of alkaline and earth alkaline ions and some metal ions on the retentions of analytes on Dowex Optipore V-493 resin were examined. Under the optimized conditions, the detection limits (3s, n = 21) for cadmium and lead were 0.43 μg L-1 and 0.65 μg L-1, respectively. The relative standard deviation (R.S.D.), and the recoveries of standard addition for this method were lower than 5% (n = 11) and 95-102%, respectively. Three standard reference samples (LGC 6010 Hard drinking water, NIST SRM 2711 Montana soil and GBW 07605 Tea) were introduced for accuracy and precision of analytical data. The proposed solid phase extraction system was successfully applied to the analysis of environmental samples

  8. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    Science.gov (United States)

    Reyes, Mariela N. Matos; Campos, Reinaldo C.

    2005-06-01

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO 3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation ( n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits ( k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l - 1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples.

  9. Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

    Science.gov (United States)

    Bibi, Aisha; Ju, Huangxian

    2016-04-01

    A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples.

  10. Atomic Absorption Spectrometric Method for Estimation of Diclofenac sodium and Mefenamic acid in Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    Sunil Jawla

    2010-01-01

    Full Text Available Diclofenac sodium and Mefenamic acid have been quantified in tablet dosage form by atomic absorption spectrometry (AAS. These methods are based on formation of the metal complexes of Diclofenac sodium and Mefenamic acid with cupric chloride and cobaltous chloride. The first method is based on reaction of both the drugs with cupric chloride to give light blue colored metal complexes, which are then extracted with dichloromethane and digested with 0.1 M nitric acid. Both the drugs are indirectly estimated via determination of copper content in the formed complexes by AAS. The second method is based on the formation of pink colored complexes of both the drugs with cobaltous chloride. These metal complexes are extracted with dichloromethane and estimated via determination of cobalt content in the formed complexes after digestion with 0.1 M nitric acid by AAS.

  11. Mass Spectrometric Detection of Bacterial Protein Toxins and Their Enzymatic Activity.

    Science.gov (United States)

    Kalb, Suzanne R; Boyer, Anne E; Barr, John R

    2015-08-31

    Mass spectrometry has recently become a powerful technique for bacterial identification. Mass spectrometry approaches generally rely upon introduction of the bacteria into a matrix-assisted laser-desorption time-of-flight (MALDI-TOF) mass spectrometer with mass spectrometric recognition of proteins specific to that organism that form a reliable fingerprint. With some bacteria, such as Bacillus anthracis and Clostridium botulinum, the health threat posed by these organisms is not the organism itself, but rather the protein toxins produced by the organisms. One such example is botulinum neurotoxin (BoNT), a potent neurotoxin produced by C. botulinum. There are seven known serotypes of BoNT, A-G, and many of the serotypes can be further differentiated into toxin variants, which are up to 99.9% identical in some cases. Mass spectrometric proteomic techniques have been established to differentiate the serotype or toxin variant of BoNT produced by varied strains of C. botulinum. Detection of potent biological toxins requires high analytical sensitivity and mass spectrometry based methods have been developed to determine the enzymatic activity of BoNT and the anthrax lethal toxins produced by B. anthracis. This enzymatic activity, unique for each toxin, is assessed with detection of the toxin-induced cleavage of strategically designed peptide substrates by MALDI-TOF mass spectrometry offering unparalleled specificity. Furthermore, activity assays allow for the assessment of the biological activity of a toxin and its potential health risk. Such methods have become important diagnostics for botulism and anthrax. Here, we review mass spectrometry based methods for the enzymatic activity of BoNT and the anthrax lethal factor toxin.

  12. Mass spectrometric immunoassay

    Science.gov (United States)

    Nelson, Randall W; Williams, Peter; Krone, Jennifer Reeve

    2007-12-04

    Rapid mass spectrometric immunoassay methods for detecting and/or quantifying antibody and antigen analytes utilizing affinity capture to isolate the analytes and internal reference species (for quantification) followed by mass spectrometric analysis of the isolated analyte/internal reference species. Quantification is obtained by normalizing and calibrating obtained mass spectrum against the mass spectrum obtained for an antibody/antigen of known concentration.

  13. An indirect atomic absorption spectrometric determination of ciprofloxacin, amoxycillin and diclofenac sodium in pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    MAHMOUD MOHAMED ISSA

    2008-05-01

    Full Text Available A highly sensitive indirect atomic absorption spectrophotometric (AAS method has been developed for the determination of very low concentrations of ciprofloxacin, amoxycillin and diclofenac sodium. The method is based on the oxidation of these drugs with iron(III. The excess of iron(III was extracted into diethyl ether and then the iron(II in the aqueous layer was aspirated into an air–acetylene flame and determined by AAS. The linear concentration ranges were 25–400, 50–500 and 60–600 ng ml-1 for ciprofloxacin, amoxycillin and diclofenac sodium, respectively. The results were statistically compared with the official method using t- and f-test at p < 0.05. There were insignificant interferences from most of the excipients present. The intra- and inter-day assay coefficients of variation were less than 6.1 % and the recoveries ranged from 95 to 103 %. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

  14. Electrothermal atomic absorption spectrometric determination of total and hexavalent chromium in atmospheric aerosols

    International Nuclear Information System (INIS)

    A method was developed which allow separate determination of Cr(VI) and total Cr from the same minute sample of atmospheric aerosols. Cr(VI) was leached was with 0.1 M Na2CO3 and the total Cr concentrations were determined after acid digestion. The method was validated by the analysis of certified reference materials, CRM 545, Mess-3 and Pacs-2 with good agreement between certified and found values. Cr concentrations in air samples taken around the chromium smelter show concentrations that exceed the maximum allowed levels in 8 h with higher values closer to the smelter. The limit of detection (LOD) of the method for Cr(VI) determination in air samples was found to be 0.2 ng m-3, i.e. lower than offered by the commonly preferred spectrophotometric and colorimetric techniques

  15. Analysis of endocrine disrupting pesticides by capillary GC with mass spectrometric detection.

    Science.gov (United States)

    Matisová, Eva; Hrouzková, Svetlana

    2012-09-01

    Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC) and fast CGC with mass spectrometric detection (MS) has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP) residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  16. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    Directory of Open Access Journals (Sweden)

    Svetlana Hrouzková

    2012-09-01

    Full Text Available Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC and fast CGC with mass spectrometric detection (MS has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important.

  17. Metabolism of boldione in humans by mass spectrometric techniques: detection of pseudoendogenous metabolites.

    Science.gov (United States)

    de la Torre, Xavier; Curcio, Davide; Colamonici, Cristiana; Molaioni, Francesco; Botrè, Francesco

    2013-01-01

    Boldione is an anabolic androgenic steroid (AAS) related to boldenone, androstenedione, and testosterone bearing two double bonds in C1 and C4 positions. Boldione is rapidly transformed to the well-known AAS boldenone, being both compounds included in the list of prohibited substances and methods published yearly by the World Anti-Doping Agency (WADA). After the administration of boldione to a male volunteer, the already described urinary metabolites of boldenone produced after reduction in C4, oxydoreduction in C3 and C17, and hydroxylation have been detected. In addition, minor new metabolites have been detected and their structure postulated after mass spectrometric analyses. Finally, the reduction of the double bound in C1 produces metabolites identical to the endogenously produced ones. A method based on gas chromatography coupled to isotope ratio mass spectrometry (GC/C/IRMS) after a urine sample purification by high performance liquid chromatography (HPLC) permitted to confirm the main synthetic like boldione/boldenone metabolite (17β-hydroxy-5β-androst-1-en-3-one) and boldenone at trace levels (synthetic or endogenous origin, and to determine the exogenous origin of metabolites with the same chemical structure of the endogenous ones. The detection of pseudoendogenous androgens of synthetic origin partially overlapped boldenone and its main metabolite detection, being an additional proof of synthetic steroids misuse. By the use of IRMS, the correct evaluation of the modifications of the steroid profile after the administration of synthetic AAS that could be converted into endogenous like ones is possible. PMID:24259377

  18. Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

    Science.gov (United States)

    Bibi, Aisha; Ju, Huangxian

    2016-04-01

    A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples. Copyright © 2016 John Wiley & Sons, Ltd. PMID:27041659

  19. Development of a cloud point extraction and preconcentration method for Cd and Ni prior to flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Manzoori, Jamshid L. [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: manzoori@tabrizu.ac.ir; Karim-Nezhad, Ghasem [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

    2004-09-13

    In this work a new cloud point extraction (CPE) methodology was developed for the separation and preconcentration of cadmium and nickel. The analyte in the initial aqueous solution was complexed with dithizone and Triton X-114 was added as surfactant. After phase separation, based on the cloud point of the mixture, and dilution of the surfactant-rich phase with tetrahydrofuran (THF), the enriched analytes were determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions and preconcentration of only 10 ml of sample in the presence of 0.05% Triton X-114, the enhancement factors of 52 and 39 and the detection limits of 0.31 {mu}g l{sup -1} and 1.2 {mu}g l{sup -1} were obtained for cadmium and nickel respectively. The proposed method was applied satisfactorily to the determination of cadmium and nickel in water samples.

  20. Mass spectrometric methods for studying nutrient mineral and trace element absorption and metabolism in humans using stable isotopes: a review

    International Nuclear Information System (INIS)

    Mass spectrometric methods for determining stable isotopes of nutrient minerals and trace elements in human metabolic studies are described and discussed. The advantages and disadvantages of the techniques of electron ionization, fast atom bombardment, thermal ionization, and inductively coupled plasma and gas chromatography mass spectrometry are evaluated with reference to their accuracy, precision, sensitivity, and convenience, and the demands of human nutrition research. Examples of specific applications are described and the significance of current developments in mass spectrometry are discussed with reference to present and probable future research needs. (Author)

  1. Determination of trace elements in Egyptian cane sugar (Deshna Factories) by neutron activation, atomic absorption spectrophotometric and inductively coupled plasma-atomic emission spectrometric analysis

    International Nuclear Information System (INIS)

    Multielement instrumental neutron activation (INAA), inductively coupled plasma-atomic emission spectrometric (ICP-AES) and atomic absorption spectrophotometric (AAS) analyses were utilized for the determination of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cu, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P, Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in sugar cane plant, raw juice, juice in different stages, syrup, deposits, molasses, A, B and C sugar, refinery 1 and 2 sugar, and in soil samples picked up from the immediate vicinity of the cane plant roots at surface, 30 and 60 cm depth, respectively. (author)

  2. Multi-element coprecipitation for separation and enrichment of heavy metal ions for their flame atomic absorption spectrometric determinations

    International Nuclear Information System (INIS)

    A preconcentration-separation technique for lead(II), cadmium(II), chromium(III), nickel(II) and manganese(II) ions has been established. The procedure is based on coprecipitation of these ions by the aid of Cu(II)-dibenzyldithiocarbamate precipitate. The precipitate was dissolved in 0.5 mL of concentrated HNO3, and made up to 5 mL with distilled water. The heavy metals were determined by flame atomic absorption spectrometer. The effects of analytical parameters like pH, amounts of reagents, sample volume, etc. on the recoveries of heavy metals were investigated. The influences of matrix ions were also examined. The detection limits for the heavy metals based on 3 sigma (N = 21) were found in the range of 0.34-0.87 μg L-1. In order to validate the proposed method, two certified reference materials of NIST SRM 2711 Montana soil and NIST SRM 1515 Apple leaves were analyzed with satisfactory results. The proposed method was applied for the determination of lead, cadmium, chromium, nickel and manganese in environmental samples

  3. Mass spectrometric detection of proteins in non-aqueous media : the case of prion proteins in biodiesel

    Energy Technology Data Exchange (ETDEWEB)

    Douma, M.D.; Kerr, G.M.; Brown, R.S.; Keller, B.O.; Oleschuk, R.D. [Queen' s Univ., Kingston, ON (Canada). Dept. of Chemistry

    2008-08-15

    This paper presented a filtration method for detecting protein traces in non-aqueous media. The extraction technique used a mixture of acetonitrile, non-ionic detergent and water along with filter disks with embedded C{sub 8}-modified silica particles to capture the proteins from non-aqueous samples. The extraction process was then followed by an elution of the protein from the filter disk and direct mass spectrometric detection and tryptic digestion with peptide mapping and MS/MS fragmentation of protein-specific peptides. The method was used to detect prion proteins in spiked biodiesel samples. A tryptic peptide with the sequence YGQGSPGGNR was used for unambiguous identification. Results of the study showed that the method is suitable for the large-scale testing of protein impurities in tallow-based biodiesel production processes. 33 refs., 6 figs.

  4. Cloud Point Extraction and Flame Atomic Absorption Spectrometric Determination of Lead, Cadmium and Palladium in Some Food and Biological Samples

    Directory of Open Access Journals (Sweden)

    M. Soylak

    2011-12-01

    Full Text Available The proposed method is based on the complexation of the Pb2+, Cd2+ and Pd2+ ions with 3-(1-(1-H-Indol-3-Yl-3-phenylallyl-1H-indole (IPAI at pH 8.0 in the presence of Triton X-114. The phase separation occured when micellar solution was heated at 55 ◦C. The surfactant-rich phase, diluted to 0.5 mL via 1.0 mol L−1 nitric acid in methanol was directly introduced into the nebulizer of the flame atomic absorption spectrometry (FAAS. Influence of variables such as pH, amount of ligand and Triton X-114, heating time and temperature were evaluated and optimized. The optimized enhancement factors for Pb2+, Cd2+ and Pd2+ ions were 22, 33 and 23, respectively and the detection limit (DLs was between of 1.6–2.6 µgL−1. The relative standard deviation (RSD of each ion was found to be less than 4.6% at 100 µgL−1. In addition, the calibration graphs were linear in the range of 0.01-0.22 μg mL−1 for Cd2+ ion, 0.018-0.26 μg mL−1 for Pb2+ ion and 0.02-0.27 μg mL−1 for Pd2+ ion with the correlation coefficients in the range of 0.995–0.999.

  5. Selective cloud point extraction and graphite furnace atomic absorption spectrometric determination of molybdenum (VI) ion in seawater samples

    Energy Technology Data Exchange (ETDEWEB)

    Filik, Hayati, E-mail: filik@istanbul.edu.tr [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey); Cengel, Tayfun; Apak, Resat [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey)

    2009-09-30

    A cloud point extraction process using the nonionic surfactant Triton X-114 to extract molybdenum from aqueous solutions was investigated. The method is based on the complexation reaction of Mo(VI) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarine: QA) and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by graphite furnace atomic absorption spectrometry (GFAAS). The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature, incubation and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the limit of detection (LOD) for Mo(VI) was 7.0 ng L{sup -1} with an preconcentration factor of {approx}25 when 10 mL of sample solution was preconcentrated to 0.4 mL. The proposed method (with extraction) showed linear calibration within the range 0.03-0.6 {mu}g L{sup -1}. The relative standard deviation (RSD) was found to be 3.7% (C{sub Mo(VI)} = 0.05 {mu}g L{sup -1}, n = 5) for pure standard solutions, whereas RSD for the recoveries from real samples ranged between 2 and 8% (mean RSD = 3.9%). The method was applied to the determination of Mo(VI) in seawater and tap water samples with a recovery for the spiked samples in the range of 98-103%. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. In order to verify the accuracy of the method, a certified reference water sample was analysed and the results obtained were in good agreement with the certified values.

  6. Flame atomic absorption spectrometric determination of trace cadmium in alloys and biological samples after solid-liquid extraction and preconcentration with use of nitroso-S

    International Nuclear Information System (INIS)

    Cadmium is quantitatively retained by 2-nitroso-1-naphthol-4-sulfonic acid (nitroso-S) and tetradecyldimethylbenzylammonium chloride (TDBA) on microcrystalline naphthalene in the pH range 5.7-10.5 from a large volumes of aqueous solutions of various samples. After filtration, the solid mass consisting of cadmium complex and naphthalene is dissolved with 5 mL of dimethylformamide and the metal was determined by flame atomic absorption spectrometric. Cadmium complex can alternatively be quantitatively adsorbed on tetradecyldimethylbenzylammonium-naphthalene adsorbent packed in a column and determined similarly. About 25 ng of cadmium can be concentrated in a column from 500 mL of aqueous sample, where its concentration is as low as 0.05 ng/mL. Eight replicate determinations of 0.1 μg/mL of cadmium in final DMF solution gave a mean absorbance of 0.060 with a relative standard deviation of 1.8 %. The sensitivity for 1 % absorption was 7.3 ng/mL. The interference of a large number of anions and cations has been studied and the optimized conditions developed were utilized for the trace determination of cadmium in various alloys and biological samples. (author)

  7. Enrichment of trace amounts of copper(II) ions in water samples using octadecyl silica disks modified by a Schiff base ionophore prior to flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Fathi, S.A.M. [Department of Chemistry, Faculty of Science, Zanjan University, PO Box 45195-313 Zanjan (Iran, Islamic Republic of); Yaftian, M.R. [Department of Chemistry, Faculty of Science, Zanjan University, PO Box 45195-313 Zanjan (Iran, Islamic Republic of)], E-mail: yaftian@znu.ac.ir

    2009-05-15

    Bis(5-bromo-2-hydroxybenzaldehyde)-1,2-propanediimine is synthesized by the reaction of 5-bromo-2-hydroxybenzaldehyde and 1,2-diaminopropane in ethanol. This ligand is used as a modifier of octadecyl silica disks for preconcentration of trace amounts of copper(II) ions, followed by nitric acid elution and flame atomic absorption spectrometric (FAAS) determination. The effect of parameters influencing the extraction efficiency, i.e. pH of the sample solutions, amount of the Schiff base, type and volume of stripping reagent, sample and eluent flow rates were evaluated. Under optimum experimental conditions, the capacity of the membrane disks modified by 4 mg of the ligand was found to be 247.7 ({+-}2.1) {mu}g of copper. The detection limit and the concentration factor of the presented method are 2.4 ng/l and greater than 400, respectively. The method was applied to the extraction, recovery and detection of copper in different synthetic and water samples.

  8. Quantitative analysis of flavonols, flavones, and flavanones in fruits, vegetables and beverages by high-performance liquid chromatography with photo-diode array and mass spectrometric detection

    DEFF Research Database (Denmark)

    Justesen, U.; Knuthsen, Pia; Leth, Torben

    1998-01-01

    A high-performance liquid chromatographic (HPLC) separation method viith photo-diode array (PDA) and mass spectrometric (MS) detection was developed to determine and quantify flavonols, flavones, and flavanones in fruits, vegetables and beverages. The compounds were analysed as aglycones, obtained...

  9. Design of Optoelectric Detection Circuit for Difference Absorption Gas Sensor

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Since the gas infrared absorption spectrum linewidth is only several nanometers occupying the source intensity of several in a thousand, it is even less than the noise of light source. The signal of gas absorption is submerged in the noise, so it is impossible to measure the concentration of gas with spectrum absorption directly. According to the principle and parameters of difference absorption system of CH4 gas, a detection circuit consisted of the lock-in amplifier is designed. The experiment results indicated that the detection circuit can satisfy the demand of the whole system, and the limit concentration is 150×10-6.

  10. Quantitative analysis of sodium di-uranate for Al, Ca, Fe, Mg, Mn, Na by flame-atomic absorption spectrometric method

    International Nuclear Information System (INIS)

    Nuclear Fuel Complex (NFC) receives Sodium Di-Uranate (SDU) from Uranium Corporation of India Limited (UCIL) for producing sinterable UO2 pellets for manufacturing fuel sub assemblies. Several impurities present in ore find their way into SDU during its conversion. Stringent specification have been laid down by the reactor designs for achieving the optimum performance of the fuel and several impurity element like Al, Ca, Fe, Mg, Mn, Na among others affects severely performance of UO2 fuel. Most of the impurity including the above mentioned elements are generally analysed by ICP-OES method. However, determination of Al, Ca, Fe, Mg, Mn and Na by ICP-OES requires lot of dilution as they are present at high levels in SDU. Apart from introducing dilution error, dilution process is very tedious and time consuming work and not a preferred choice in an industrial lab like control lab where large analytical load exists and time bound analysis is a requirement. To avoid these difficulties a simple and reliable Flame Atomic absorption spectrometric technique has been developed for regular analysis. Present method involves dissolution of SDU sample in Conc. HNO3 and after the complete dissolution the sample solution has been evaporated to near dryness on a hot plate. Subsequently sample solution has been brought into 4N HNO3 medium

  11. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

    2013-01-01

    A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

  12. Thermally detected optical absorption in sophisticated nitride structures

    Energy Technology Data Exchange (ETDEWEB)

    Vasson, A.; Leymarie, J. [LASMEA-UMR 6602 CNRS-UBP, 63177 Aubiere Cedex (France); Shubina, T.V. [Ioffe Physico-Technical Institute, RAS, St. Petersburg 194021 (Russian Federation)

    2005-02-01

    The thermally detected optical absorption (TDOA) is applied to elucidate peculiarities of absorption in nitride structures of unusual morphology like GaN nanocolumns or InN layers with various imperfections. A study of GaN structures permits us to establish position of an absorption edge in TDOA spectra. We demonstrate that the absorption edge is different in GaN regions of opposite polarities. In InN with metallic In inclusions, this technique enable separation of InN interband absorption and extinction related to the Mie resonances, if the latter are below the principal absorption edge. (copyright 2005 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  13. Standard test method for graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2000-01-01

    1.1 This test method covers procedures for using graphite furnace atomic absorption spectroscopy (GFAAS) to quantitatively determine lead and cadmium extracted by acetic acid at room temperature from the food-contact surface of foodware. The method is applicable to food-contact surfaces composed of silicate-based materials (earthenware, glazed ceramicware, decorated ceramicware, decorated glass, and lead crystal glass) and is capable of determining lead concentrations greater than 0.005 to 0.020 g/mL and cadmium concentrations greater than 0.0005 to 0.002 g/mL, depending on instrument design. 1.2 This test method also describes quality control procedures to check for contamination and matrix interference during GFAAS analyses and a specific sequence of analytical measurements that demonstrates proper instrument operation during the time period in which sample solutions are analyzed. 1.3 Cleaning and other contamination control procedures are described in this test method. Users may modify contamination cont...

  14. Capillary liquid chromatography using laser-based and mass spectrometric detection. Final technical progress report, September 1, 1989--January 31, 1993

    Energy Technology Data Exchange (ETDEWEB)

    Sepaniak, M.J.; Cook, K.D.

    1992-09-01

    In the years following the 1986 seminal paper (J. Chromatogr. Sci., 24, 347-352) describing modern capillary zone electrophoresis (CZE), the prominence of capillary electrokinetic separation techniques has grown. A related electrochromatographic technique is micellar electrokinetic capillary chromatography (MECC). This report presents a brief synopsis of research efforts during the current 3-year period. In addition to a description of analytical separations-based research, results of efforts to develop and expand spectrometric detection for the techniques is reviewed. Laser fluorometric detection schemes have been successfully advanced. Mass spectrometric research was less fruitful, largely owing to personnel limitations. A regenerable fiber optic sensor was developed that can be used to remotely monitor chemical carcinogens, etc. (DLC)

  15. Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

    1997-01-01

    An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination...... with an aqueous solution of 6 mmol L-1 of salicylate ion at pH 8.5 as the mobile phase which allowed the isocratic separation of the four selenium analytes within 8 minutes. The separated selenium species were detected on-line by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma mass...

  16. Simultaneous Preconcentration of Copper, Nickel, Cobalt and Lead Ions Prior to Their Flame Atomic Absorption Spectrometric Determination

    International Nuclear Information System (INIS)

    A sensitive and simple method for the simultaneous preconcentration of nutritionally important minerals in real samples has been reported. The method is based on the adsorption of Cu2+, Ni2+, Co2+ and Pb2+ on 4-propyl-2-thiouracil (PUT) loaded on activated carbon. The metals on the complexes are eluted using 5 mL 3 M HNO3 in acetone. The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally higher than 95 %. The detection limits for Cu2+, Ni2+, Co2+ and Pb2+ were 1.6, 1.3, 1.2, 2.3 ng ml-1, respectively. The method has been successfully applied for these metals content evaluation in some real samples including natural water samples

  17. A Mass Spectrometric Analysis Method Based on PPCA and SVM for Early Detection of Ovarian Cancer

    Directory of Open Access Journals (Sweden)

    Jiang Wu

    2016-01-01

    Full Text Available Background. Surfaced-enhanced laser desorption-ionization-time of flight mass spectrometry (SELDI-TOF-MS technology plays an important role in the early diagnosis of ovarian cancer. However, the raw MS data is highly dimensional and redundant. Therefore, it is necessary to study rapid and accurate detection methods from the massive MS data. Methods. The clinical data set used in the experiments for early cancer detection consisted of 216 SELDI-TOF-MS samples. An MS analysis method based on probabilistic principal components analysis (PPCA and support vector machine (SVM was proposed and applied to the ovarian cancer early classification in the data set. Additionally, by the same data set, we also established a traditional PCA-SVM model. Finally we compared the two models in detection accuracy, specificity, and sensitivity. Results. Using independent training and testing experiments 10 times to evaluate the ovarian cancer detection models, the average prediction accuracy, sensitivity, and specificity of the PCA-SVM model were 83.34%, 82.70%, and 83.88%, respectively. In contrast, those of the PPCA-SVM model were 90.80%, 92.98%, and 88.97%, respectively. Conclusions. The PPCA-SVM model had better detection performance. And the model combined with the SELDI-TOF-MS technology had a prospect in early clinical detection and diagnosis of ovarian cancer.

  18. Cloud point extraction and flame atomic absorption spectrometric determination of trace lead in freshwater fish%浊点萃取-火焰原子吸收光谱法测定淡水鱼中痕量铅

    Institute of Scientific and Technical Information of China (English)

    王秀峰; 李龙; 张春丽; 林朋; 崔书亚

    2012-01-01

    采用以双硫腙为络合剂、Triton X- 100为表面活性剂的新型浊点萃取体系富集淡水鱼中的痕量铅,并用火焰原子吸收光谱法对其进行测定.探讨了溶液pH、表面活性剂浓度、络合剂用量、平衡温度、平衡时间等对浊点萃取及测定灵敏度的影响,优化了实验条件.在最佳条件下测得铅的检出限为0.090μg/L,校准曲线相关系数为0.9999.该方法已用于淡水鱼中痕量铅的测定.%A new cloud point extraction-flame atomic absorption spectrometric method has been developed to determine trace lead. Dithizone was selected as the complex reagent and Triton X - 100 as the surfactant. Effects of pH, concentrations of surfactant and complex reagent, equilibrium temperature and time on the efficiency and sensitivity of cloud point extraction were investigated. Under optimal conditions, the calibration curve was linear over the concentration range of 0. 1 - 60μg/L with correlation coefficient of 0. 9999 and detection limit of 0. 090 μg/L. The present method was applied to the determination of trace lead in freshwater fish samples with satisfactory results.

  19. MALDI-TOF mass spectrometric detection of multiplex single base extended primers

    DEFF Research Database (Denmark)

    Mengel-From, Jonas; Sanchez Sanchez, Juan Jose; Børsting, Claus;

    2004-01-01

    One of the most promising techniques for typing of multiple single-nucleotide polymorphism (SNP) is detection of single base extension primers (SBE) by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). We present a new MALDI-TOF MS protocol for typing...

  20. Mass Spectrometric Detection of Botulinum Neurotoxin by Measuring its Activity in Serum and Milk

    Science.gov (United States)

    Kalb, Suzanne R.; Pirkle, James L.; Barr, John R.

    Botulinum neurotoxins (BoNTs) are bacterial protein toxins which are considered likely agents for bioterrorism due to their extreme toxicity and high availability. A new mass spectrometry based assay called Endopep MS detects and defines the toxin serotype in clinical and food matrices via toxin activity upon a peptide substrate which mimics the toxin's natural target. Furthermore, the subtype of the toxin is differentiated by employing mass spectrometry based proteomic techniques on the same sample. The Endopep-MS assay selectively detects active BoNT and defines the serotype faster and with sensitivity greater than the mouse bioassay. One 96-well plate can be analyzed in under 7 h. On higher level or "hot" samples, the subtype can then be differentiated in less than 2 h with no need for DNA.

  1. A small azide-modified thiazole-based reporter molecule for fluorescence and mass spectrometric detection

    Directory of Open Access Journals (Sweden)

    Stefanie Wolfram

    2014-10-01

    Full Text Available Molecular probes are widely used tools in chemical biology that allow tracing of bioactive metabolites and selective labeling of proteins and other biomacromolecules. A common structural motif for such probes consists of a reporter that can be attached by copper(I-catalyzed 1,2,3-triazole formation between terminal alkynes and azides to a reactive headgroup. Here we introduce the synthesis and application of the new thiazole-based, azide-tagged reporter 4-(3-azidopropoxy-5-(4-bromophenyl-2-(pyridin-2-ylthiazole for fluorescence, UV and mass spectrometry (MS detection. This small fluorescent reporter bears a bromine functionalization facilitating the automated data mining of electrospray ionization MS runs by monitoring for its characteristic isotope signature. We demonstrate the universal utility of the reporter for the detection of an alkyne-modified small molecule by LC–MS and for the visualization of a model protein by in-gel fluorescence. The novel probe advantageously compares with commercially available azide-modified fluorophores and a brominated one. The ease of synthesis, small size, stability, and the universal detection possibilities make it an ideal reporter for activity-based protein profiling and functional metabolic profiling.

  2. Transient C IV Broad Absorption Lines in radio detected QSOs

    CERN Document Server

    Vivek, M; Gupta, N

    2015-01-01

    We study the transient (i.e. emerging or disappearing) C IV broad absorption line (BAL) components in 50 radio detected QSOs using multi-epoch spectra available in Sloan Digital Sky Survey DR10. We report the detectionof 6 BALQSOs having at least one distinct transient C IV absorption component. Based on the structure function analysis of optical light curves, we suggest that the transient absorption is unlikely to be triggered by continuum variations. Transient absorption components usually have low C IV equivalent widths ( 10000 \\kms) and typically occur over rest-frame timescales > 800 days. The detection rate of transient C IV absorption seen in our sample is higher than that reported in the literature. Using a control sample of QSOs, we show that this difference is most likely due to the longer monitoring time-scale of sources in our sample while the effect of small number statistics cannot be ignored. Thus, in order to establish the role played by radio jets in driving the BAL outflows, we need a larger...

  3. Graphite furnace and hydride generation atomic absorption spectrometric determination of cadmium, lead, and tin traces in natural surface waters: Study of preconcentration technique performance

    International Nuclear Information System (INIS)

    In this study three major types of preconcentration methods based upon different principles (cation exchange, physical absorption and hydrophobic extraction) were evaluated and optimized for the extraction and determination of three highly toxic heavy metals namely Cd, Pb and Sn by graphite furnace and hybrid generation atomic absorption spectrometry in real samples. The optimum analytical conditions were examined and the analytical features of each method were revealed and compared. Detection limits as low as 0.003-0.025 μg L-1 for Cd2+, 0.05-0.10 μg L-1 for Pb2+ and 0.1-0.25 μg L-1 for Sn4+ depending on the extraction method were obtained with RSD values between 3.08% and 6.11%. A preliminary assessment of the pollution status of three important natural ecosystems in Epirus region (NW Greece) was performed and some early conclusions were drawn and discussed

  4. Simulation for photon detection in spectrometric system of high purity (HPGe) using MCNPX code

    International Nuclear Information System (INIS)

    The Brazilian National Commission of Nuclear Energy defines parameters for classification and management of radioactive waste in accordance with the activity of materials. The efficiency of a detection system is crucial to determine the real activity of a radioactive source. When it's possible, the system's calibration should be performed using a standard source. Unfortunately, there are only a few cases that it can be done this way, considering the difficulty of obtaining appropriate standard sources for each type of measurement. So, computer simulations can be performed to assist in calculating of the efficiency of the system and, consequently, also auxiliary the classification of radioactive waste. This study aims to model a high purity germanium (HPGe) detector with MCNPX code, approaching the spectral values computationally obtained of the values experimentally obtained for the photopeak of 137Cs. The approach will be made through changes in outer dead layer of the germanium crystal modeled. (author)

  5. Flame Atomic Absorption Spectrometric Determination of Trace Amounts of Silver after Solid-Phase Extraction with 2-Mercaptobenzothiazole Immobilized on Microcrystalline Naphthalene

    Directory of Open Access Journals (Sweden)

    Farid Shakerian

    2013-01-01

    Full Text Available A simple and sensitive solid-phase extraction (SPE procedure combined with flame atomic absorption spectrometry (FAAS was designed for the extraction and determination of trace amounts of silver. A column of immobilized 2-mercaptobenzothiazole (MBT on microcrystalline naphthalene was used as the sorbent. Silver was quantitatively retained on the column in the pH range of 0.5–6.0. After extraction, the solid mass consisting of silver complex and naphthalene was dissolved out of the column with 5.0 mL of dimethylformamide, and the analyte was determined by flame atomic absorption spectrometry (FAAS. Under the optimum experimental conditions, the adsorption capacity was found to be 1.18 mg of silver per gram of the sorbent. A sample volume of 800 mL resulted in a preconcentration factor of 160. The relative standard deviation obtained for ten replicate determinations at a concentration of 0.8 µg L−1 was 1.4%, and the limit of detection was 0.02 µg L−1. The method was successfully applied to the determination of silver in radiology film, waste water, and natural water samples. The accuracy was examined by recovery experiments, independent analysis by electrothermal atomic absorption spectrometry, and analysis of two certified reference materials.

  6. Flame atomic absorption spectrometric determination of trace quantities of cadmium in water samples after cloud point extraction in Triton X-114 without added chelating agents

    Energy Technology Data Exchange (ETDEWEB)

    Afkhami, Abbas [Department of Chemistry, Faculty of Science, Bu-Ali Sina University, Hamadan (Iran, Islamic Republic of)]. E-mail: afkhami@basu.ac.ir; Madrakian, Tayyebeh [Department of Chemistry, Faculty of Science, Bu-Ali Sina University, Hamadan (Iran, Islamic Republic of); Siampour, Hajar [Department of Chemistry, Faculty of Science, Bu-Ali Sina University, Hamadan (Iran, Islamic Republic of)

    2006-11-16

    A new micell-mediated phase separation method for preconcentration of ultra-trace quantities of cadmium as a prior step to its determination by flame atomic absorption spectrometry has been developed. The method is based on the cloud point extraction (CPE) of cadmium in iodide media with Triton X-114 in the absence of any chelating agent. The optimal extraction and reaction conditions (e.g., acid concentration, iodide concentration, effect of time) were studied, and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and improvement factors) were obtained. Linearity was obeyed in the range of 3-300 ng mL{sup -1} of cadmium. The detection limit of the method is 1.0 ng mL{sup -1} of cadmium. The interference effect of some anions and cations was also tested. The method was applied to the determination of cadmium in tap water, waste water, and sea water samples.

  7. Searching for Dark Absorption with Direct Detection Experiments

    OpenAIRE

    Bloch, Itay M.; Essig, Rouven(C.N. Yang Institute for Theoretical Physics, Stony Brook University, Stony Brook, NY, 11794, U.S.A.); Tobioka, Kohsaku; Volansky, Tomer; Yu, Tien-Tien

    2016-01-01

    We consider the absorption by bound electrons of dark matter in the form of dark photons and axion-like particles, as well as of dark photons from the Sun, in current and next-generation direct detection experiments. Experiments sensitive to electron recoils can detect such particles with masses between a few eV to more than 10 keV. For dark photon dark matter, we update a previous bound based on XENON10 data and derive new bounds based on data from XENON100 and CDMSlite. We find these experi...

  8. Anti-aggregation-based spectrometric detection of Hg(II) at physiological pH using gold nanorods.

    Science.gov (United States)

    Rajeshwari, A; Karthiga, D; Chandrasekaran, Natarajan; Mukherjee, Amitava

    2016-10-01

    An efficient detection method for Hg (II) ions at physiological pH (pH7.4) was developed using tween 20-modified gold nanorods (NRs) in the presence of dithiothreitol (DTT). Thiol groups (-SH) at the end of DTT have a higher affinity towards gold atoms, and they can covalently interact with gold NRs and leads to their aggregation. The addition of Hg(II) ions prevents the aggregation of gold NRs due to the covalent bond formation between the -SH group of DTT and Hg(II) ions in the buffer system. The changes in the longitudinal surface plasmon resonance peak of gold NRs were characterized using a UV-visible spectrophotometer. The absorption intensity peak of gold NRs at 679nm was observed to reduce after interaction with DTT, and the absorption intensity was noted to increase by increasing the concentration of Hg(II) ions. The TEM analysis confirms the morphological changes of gold NRs before and after addition of Hg(II) ions in the presence of DTT. Further, the aggregation and disaggregation of gold NRs were confirmed by particle size and zeta potential analysis. The developed method shows an excellent linearity (y=0.001x+0.794) for the graph plotted between the absorption ratio and Hg(II) concentration (1 to 100pM) under the optimized conditions. The limit of detection was noted to be 0.42pM in the buffer system. The developed method was tested in simulated body fluid, and it was found to have a good recovery rate. PMID:27287171

  9. Atomic absorption spectrometric determination of some metal ions after preconcentration by solid phase extraction using amberlite XAD 16 resin loaded with thenoyltrifluoroacetone

    International Nuclear Information System (INIS)

    Complete text of publication follows. The direct determination of extremely low concentrations of trace elements by modern atomic spectroscopic methods, such as atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry is often difficult because of insufficient sensitivity and selectivity of the methods used. For this reason, the preliminary separation and preconcentration of trace elements from the matrix are often required. Solid phase extraction shows several major advantages such as simplicity, rapidity and high enrichment factor, the ability of combination with different detection techniques in the form of on-line or off-line mode and finally cost saving (Tokalioglu et al., Microchim Acta 164 (2009) 471-477.). A new solid phase extraction method for the separation and preconcentration of Cu(II), Pb(II), Ni(II), Co(II), Mn(II) and Fe(III) ions was developed. As solid phase material, Amberlite XAD-16 resin loaded with thenoyltrifluoroacetone (TTA) was used. For this purpose, 0.5 g of the resin was saturated with 10 mL of 0.5% (w/v) TTA solution. After preconcentrating, the metals retained on the resin were eluted with 10 mL of 2 mol L-1 HCl and then determined by flame atomic absorption spectrometry. The effect of some parameters for the preconcentration of the metal ions was investigated. The optimum pH was found as 6. Eluent for quantitative elution was 10 mL of 2 mol L-1 HCl.

  10. Selective cloud point extraction and preconcentration of trace amounts of silver as a dithizone complex prior to flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Manzoori, Jamshid L.; Karim-Nezhad, Ghasem

    2003-05-19

    Dithizone (diphenylthiocarbazone) was used as a complexing agent in cloud point extraction for the first time and applied for selective preconcentration of trace amounts of silver. The analyte in the initial aqueous solution was acidified with sulfuric acid (pH<1) and Triton X-114 was added as a surfactant. After phase separation, based on the cloud point separation of the mixture, the surfactant rich phase was diluted with tetrahydrofuran (THF) and the analyte determined in the enriched solution by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, a preconcentration factor of 43 was obtained for only 10 ml of sample. The analytical curve was linear in the range of 3-200 ng ml{sup -1} and the limit of detection was 0.56 ng ml{sup -1}. The proposed method was applied to the determination of silver in water samples.

  11. On-line preconcentration of cobalt in drinking water using a minicolumn packed with activated carbon coupled to electrothermal atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Cerutti, Soledad; Moyano, Susana; Gasquez, Jose A.; Stripeikis, Jorge; Olsina, Roberto A.; Martinez, Luis D. E-mail: ldm@unsl.edu.ar

    2003-11-21

    An on-line flow injection preconcentration-electrothermal atomic absorption spectrometry method is developed for trace determination of cobalt in drinking water samples by sorption on a conical minicolumn packed with activated carbon at pH 9.5. The cobalt was eluted from the minicolumn with 10% (v/v) nitric acid. An enrichment factor of 190-fold for a sample volume of 10 ml was obtained. The detection limit (DL) value for the preconcentration method proposed was 5 ng l{sup -1}. The precision for 10 replicate determinations at the 50 ng l{sup -1} Co level was 4.7% relative standard deviation. The calibration graph using the preconcentration system for cobalt was linear with a correlation coefficient of 0.9993 at levels near the DLs up to at least 0.35 {mu}g l{sup -1}. The method was successfully applied to the determination of cobalt in drinking water samples.

  12. Detecting ultralight bosonic dark matter via absorption in superconductors

    Science.gov (United States)

    Hochberg, Yonit; Lin, Tongyan; Zurek, Kathryn M.

    2016-07-01

    Superconducting targets have recently been proposed for the direct detection of dark matter as light as a keV, via elastic scattering off conduction electrons in Cooper pairs. Detecting such light dark matter requires sensitivity to energies as small as the superconducting gap of O (meV ). Here we show that these same superconducting devices can detect much lighter DM, of meV to eV mass, via dark matter absorption on a conduction electron, followed by emission of an athermal phonon. We demonstrate the power of this setup for relic kinetically mixed hidden photons, pseudoscalars, and scalars, showing that the reach can exceed current astrophysical and terrestrial constraints with only a moderate exposure.

  13. Detecting Ultralight Bosonic Dark Matter via Absorption in Superconductors

    CERN Document Server

    Hochberg, Yonit; Zurek, Kathryn M

    2016-01-01

    Superconducting targets have recently been proposed for the direct detection of dark matter as light as a keV, via elastic scattering off conduction electrons in Cooper pairs. Detecting such light dark matter requires sensitivity to energies as small as the superconducting gap of O(meV). Here we show that these same superconducting devices can detect much lighter DM, of meV to eV mass, via dark matter absorption on a conduction electron, followed by emission of an athermal phonon. We demonstrate the power of this setup for relic kinetically mixed hidden photons, pseudoscalars, and scalars, showing the reach can exceed current astrophysical and terrestrial constraints with only a moderate exposure.

  14. Determination of Palladium in Resin by Lead Fire Assaying-Flame Atomic Absorption Spectrometric Method%铅试金富集-火焰原子吸收光谱法测定树脂中钯

    Institute of Scientific and Technical Information of China (English)

    王芳; 陈小兰; 林海山; 李小玲; 肖红新

    2013-01-01

    通过铅试金富集树脂中的钯并用银作钯灰吹保护,得到的银钯合粒用王水溶解,在5%的盐酸介质中,采用原子吸收光谱法测定钯,该法测钯的相对标准偏差RSD为0.53%,加标回收率在99.04%~100.10%之间。%Palladium in resin was enriched by lead assaying, using silver as a protective agent to produce silver-palladium alloy, and then the alloy was dissolved in aqua regia. Air acetylene flame atomic absorption spectrometric method was used to determinate palladium in 5%hydrochloric acid solution. The relative standard deviation (RSD) in determination of palladium is 0.53%and the recovery rate is between 99.04%~100.10%.

  15. Are cold flows detectable with metal absorption lines?

    CERN Document Server

    Kimm, Taysun; Devriendt, Julien; Pichon, Christophe

    2010-01-01

    [Abridged] Cold gas flowing within the "cosmic web" is believed to be an important source of fuel for star formation at high redshift. However, the presence of such filamentary gas has never been observationally confirmed. In this work, we investigate in detail whether such cold gas is detectable using low-ionisation metal absorption lines, such as CII \\lambda1334 as this technique has a proven observational record for detecting gaseous structures. Using a large statistical sample of galaxies from the Mare Nostrum N-body+AMR cosmological simulation, we find that the typical covering fraction of the dense, cold gas in 10^12 Msun haloes at z~2.5 is lower than expected (~5%). In addition, the absorption signal by the interstellar medium of the galaxy itself turns out to be so deep and so broad in velocity space that it completely drowns that of the filamentary gas. A detectable signal might be obtained from a cold filament exactly aligned with the line of sight, but this configuration is so unlikely that it woul...

  16. Are cold flows detectable with metal absorption lines?

    Science.gov (United States)

    Kimm, Taysun; Slyz, Adrianne; Devriendt, Julien; Pichon, Christophe

    2011-05-01

    Cosmological simulations have shown that dark matter haloes are connected to each other by large-scale filamentary structures. Cold gas flowing within this ‘cosmic web’ is believed to be an important source of fuel for star formation at high redshift. However, the presence of such filamentary gas has never been observationally confirmed despite the fact that its covering fraction within massive haloes at high redshift is predicted to be significant (˜25 per cent). In this Letter, we investigate in detail whether such cold gas is detectable using low-ionization metal absorption lines, such as C IIλ1334, as this technique has a proven observational record for detecting gaseous structures. Using a large statistical sample of galaxies from the MARENOSTRUM N-body+ adaptive mesh refinement (AMR) cosmological simulation, we find that the typical covering fraction of the dense, cold gas in 1012 M⊙ haloes at z˜ 2.5 is lower than expected (˜5 per cent). In addition, the absorption signal by the interstellar medium of the galaxy itself turns out to be so deep and so broad in velocity space that it completely drowns that of the filamentary gas. A detectable signal might be obtained from a cold filament exactly aligned with the line of sight, but this configuration is so unlikely that it would require surveying an overwhelmingly large number of candidate galaxies to tease it out. Finally, the predicted metallicity of the cold gas in filaments is extremely low (≤10-3 Z⊙). If this result persists when higher resolution runs are performed, it would significantly increase the difficulty of detecting filamentary gas inflows using metal lines. However, even if we assume that filaments are enriched to Z⊙, the absorption signal that we compute is still weak. We are therefore led to conclude that it is extremely difficult to observationally prove or disprove the presence of cold filaments as the favourite accretion mode of galaxies using low-ionization metal absorption

  17. Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A., E-mail: joseph.caruso@uc.edu; Landero-Figueroa, Julio

    2014-10-01

    The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV–VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag{sup +}) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg{sup −1} detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

  18. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

    A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium.

  19. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

    A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. PMID:26041239

  20. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples

    International Nuclear Information System (INIS)

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL-1 for Cd2+, Pb2+, Pd2+ and Ag+ along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd2+, Pb2+, Pd2+ and Ag+, respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.

  1. A biosorption system for metal ions on Penicillium italicum - loaded on Sepabeads SP 70 prior to flame atomic absorption spectrometric determinations

    International Nuclear Information System (INIS)

    A solid phase extraction (SPE) preconcentration system, coupled to a flame atomic absorption spectrometer (FAAS), was developed for the determination of copper(II), cadmium(II), lead(II), manganese(II), iron(III), nickel(II) and cobalt(II) ions at the μg L-1 levels on Penicillium italicum - loaded on Sepabeads SP 70. The analytes were adsorbed on biosorbent at the pH range of 8.5-9.5. The adsorbed metals were eluted with 1 mol L-1 HCl. The influences of the various analytical parameters including pH of the aqueous solutions, sample volume, flow rates were investigated for the retentions of the analyte ions. The recovery values are ranged from 95-102%. The influences of alkaline, earth alkaline and some transition metal ions were also discussed. Under the optimized conditions, the detection limits (3 s, n = 21) for analytes were in the range of 0.41 μg L-1 (cadmium) and 1.60 μg L-1 (iron). The standard reference materials (IAEA 336 Lichen, NIST SRM 1573a Tomato leaves) were analyzed to verify the proposed method. The method was successfully applied for the determinations of analytes in natural water, cultivated mushroom, lichen (Bryum capilare Hedw), moss (Homalothecium sericeum) and refined table salt samples

  2. Development of on-line single-drop micro-extraction sequential injection system for electrothermal atomic absorption spectrometric determination of trace metals

    International Nuclear Information System (INIS)

    A novel automatic sequential injection (SI) single-drop micro-extraction (SDME) system is proposed as versatile approach for on-line metal preconcentration and/or separation. Coupled to electrothermal atomic absorption spectrometry (ETAAS) the potentials of this SI scheme are demonstrated for trace cadmium determination in water samples. A non-charged complex of cadmium with ammonium diethyldithiophosphate (DDPA) was produced and extracted on-line into a 60 μL micro-drop of di-isobutyl ketone (DIBK). The extraction procedure was performed into a newly designed flow-through extraction cell coupled on a sequential injection manifold. As the complex Cd(II)-DDPA flowed continuously around the micro-droplet, the analyte was extracting into the solvent micro-drop. All the critical parameters were optimized and offered good performance characteristics and high preconcentration ratios. For 600 s micro-extraction time, the enhancement factor was 10 and the sampling frequency was 6 h-1. The detection limit was 0.01 μg L-1 and the precision (RSD at 0.1 μg L-1 of cadmium) was 3.9%. The proposed method was evaluated by analyzing certified reference material

  3. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, Mehrorang, E-mail: m_ghaedi@mail.yu.ac.ir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Shokrollahi, Ardeshir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Niknam, Khodabakhsh [Chemistry Department, Persian Gulf University, Bushehr (Iran, Islamic Republic of); Niknam, Ebrahim; Najibi, Asma [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2009-09-15

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL{sup -1} for Cd{sup 2+}, Pb{sup 2+}, Pd{sup 2+} and Ag{sup +} along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd{sup 2+}, Pb{sup 2+}, Pd{sup 2+} and Ag{sup +}, respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.

  4. Use of sodium tungstate as a permanent chemical modifier for slurry sampling electrothermal atomic absorption spectrometric determination of indium in soils

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, Ignacio; Rivas, Ricardo E.; Hernandez-Cordoba, Manuel [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    A number of chemical modifiers have been assessed for the direct determination of indium in soils using electrothermal atomic absorption spectrometry and slurry sampling. The best results were obtained when the graphite atomizer was impregnated with sodium tungstate, which acts as a permanent chemical modifier. Slurries were prepared by suspending 100 mg sample in a solution containing 1% (v/v) concentrated nitric acid and 10% (v/v) concentrated hydrofluoric acid and then 15-{mu}L aliquots were directly introduced into the atomizer. Standard indium solutions prepared in the suspension medium in the range 4-80 {mu}g L{sup -1} indium were used for calibration. The relative standard deviation for ten consecutive measurements of a 40 {mu}g L{sup -1} indium solution was 2.8%. The limit of detection in soils was 0.1 {mu}g g{sup -1}. The reliability of the procedures was confirmed by analysing two standard reference materials and by using an alternative procedure. (orig.)

  5. Searching for Dark Absorption with Direct Detection Experiments

    CERN Document Server

    Bloch, Itay M; Tobioka, Kohsaku; Volansky, Tomer; Yu, Tien-Tien

    2016-01-01

    We consider the absorption by bound electrons of dark matter in the form of dark photons and axion-like particles, as well as of dark photons from the Sun, in current and next-generation direct detection experiments. Experiments sensitive to electron recoils can detect such particles with masses between a few eV to more than 10 keV. For dark photon dark matter, we update a previous bound based on XENON10 data and derive new bounds based on data from XENON100 and CDMSlite. We find these experiments to disfavor previously allowed parameter space. Moreover, we derive sensitivity projections for SuperCDMS at SNOLAB for silicon and germanium targets, as well as for various possible experiments with scintillating targets (cesium iodide, sodium iodide, and gallium arsenide). The projected sensitivity can probe large new regions of parameter space. For axion-like particles, the same current direction detection data improves on previously known direct-detection constraints but does not bound new parameter space beyond...

  6. Stable isotope dilution analysis of salicylic acid and hydroquinone in human skin samples by gas chromatography with mass spectrometric detection.

    Science.gov (United States)

    Judefeind, Anja; van Rensburg, Peet Jansen; Langelaar, Stephan; du Plessis, Jeanetta

    2007-06-01

    A sensitive and accurate gas chromatographic-mass spectrometric (GC-MS) method has been developed for the quantitative determination of salicylic acid (SA) and hydroquinone (HQ) from human skin samples and cosmetic emulsions. Deuterium labeled SA-d(6) and HQ-d(6) were used as internal standards (IS). The samples were extracted with methanol, dried under nitrogen and derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)+1% trimethylchlorosilane (TMCS). Quantification was performed in SIM mode with a limit of quantification (LOQ) of 50 ng ml(-1) for SA and 10 ng ml(-1) for HQ. The inter-day variation (R.S.D.) was less than 5% and the accuracy was better than 13.3% for both compounds. The recoveries from the different matrices ranged between 93.1 and 103.3% for SA, and 97.3 and 100.8% for HQ.

  7. Detection of electron paramagnetic resonance absorption using frequency modulation

    Science.gov (United States)

    Hirata, Hiroshi; Kuyama, Toshifumi; Ono, Mitsuhiro; Shimoyama, Yuhei

    2003-10-01

    A frequency modulation (FM) method was developed to measure electron paramagnetic resonance (EPR) absorption. The first-derivative spectrum of 1,1-diphenyl-2-picrylhydrazyl (DPPH) powder was measured with this FM method. Frequency modulation of up to 1.6 MHz (peak-to-peak) was achieved at a microwave carrier frequency of 1.1 GHz. This corresponds to a magnetic field modulation of 57 μT (peak-to-peak) at 40.3 mT. By using a tunable microwave resonator and automatic control systems, we achieved a practical continuous-wave (CW) EPR spectrometer that incorporates the FM method. In the present experiments, the EPR signal intensity was proportional to the magnitude of frequency modulation. The background signal at the modulation frequency (1 kHz) for EPR detection was also proportional to the magnitude of frequency modulation. An automatic matching control (AMC) system reduced the amplitude of noise in microwave detection and improved the baseline stability. Distortion of the spectral lineshape was seen when the spectrometer settings were not appropriate, e.g., with a lack of the open-loop gain in automatic tuning control (ATC). FM is an alternative to field modulation when the side-effect of field modulation is detrimental for EPR detection. The present spectroscopic technique based on the FM scheme is useful for measuring the first derivative with respect to the microwave frequency in investigations of electron-spin-related phenomena.

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

    Science.gov (United States)

    Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

    2009-06-30

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

  9. Electrothermal atomic absorption spectrometric determination of cadmium and lead in traces in aquatic systems following flotation by two chromium(III) collectors.

    Science.gov (United States)

    Kormusoska, Natasa Bakreska; Cundeva, Katarina; Stafilov, Trajce

    2009-10-01

    A fast flotation method for determination of cadmium and lead in aquatic systems by two chromium(III) collectors is described. The first collector is a colloid precipitate of hydrated chromium(III) oxide, Cr2O3 x xH2O, while the second is a bulk chromium(III) pentamethylenedithiocarbamate, Cr(PMDTC)3. Cadmium and lead present in water are incorporated into the collector mass at pH 7.5 by addition of 20 mg of Cr(III) and 0.4 mmol of pentamethyleneammonium pentamethylenedithiocarbamate, PMA-PMDTC, to 0.5 L water sample. A solid precipitate was separated from the processed water system by air bubbles. After dissolving with strong acid, the solution is tested by electrothermal atomic absorption spectrometry (ETAAS). The limit of detection for Cd by flotation/ETAAS method is 0.002 microg L(-1), while for Pb is 0.04 microg L(-1). The precision of the method is expressed as relative standard deviations ranging of 5.0% for Cd (concentration range from 0.1 to 0.5 microg L(-1)) and 4.25% for Pb (concentration range from 0.5 to 5 microg L(-1)). The characteristic mass (mass that gives an integrated absorbance of 0.0044 s) of 1.06 pg for Cd and 16.7 pg for Pb were obtained. The method was validated by the standard additions and by its application to the reference materials (Surface water-SPS-SW-1, River Thames Water-LGC-6019). PMID:19847715

  10. Novel analytical reagent for the application of cloud-point preconcentration and flame atomic absorption spectrometric determination of nickel in natural water samples

    Energy Technology Data Exchange (ETDEWEB)

    Suvardhan, K. [Environmental Monitoring Laboratory, Department of Chemistry, S.V. University, AP (India); Rekha, D. [Environmental Monitoring Laboratory, Department of Chemistry, S.V. University, AP (India); Kumar, K. Suresh [Environmental Monitoring Laboratory, Department of Chemistry, S.V. University, AP (India); Prasad, P. Reddy [Environmental Monitoring Laboratory, Department of Chemistry, S.V. University, AP (India); Kumar, J. Dilip [Environmental Monitoring Laboratory, Department of Chemistry, S.V. University, AP (India); Jayaraj, B. [Department of Mathematics, S.V. University, Tirupati 517502, AP (India); Chiranjeevi, P. [Environmental Monitoring Laboratory, Department of Chemistry, S.V. University, AP (India)]. E-mail: chiranjeevipattium@gmail.com

    2007-06-01

    Cloud-point extraction was applied as a preconcentration of nickel after formation of complex with newly synthesized N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13] pentaoxacyclopentadecin-15-yl-methanimine, and later determined by flame atomic absorption spectrometry (FAAS) using octyl phenoxy polyethoxy ethanol (Triton X-114) as surfactant. Nickel was complexed with N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12 octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine in an aqueous phase and was kept for 15 min in a thermo-stated bath at 40 deg. C. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. The chemical variables affecting the cloud-point extraction were evaluated, optimized and successfully applied to the nickel determination in various water samples. Under the optimized conditions, the preconcentration system of 100 ml sample permitted an enhancement factor of 50-fold. The detailed study of various interferences made the method more selective. The detection limits obtained under optimal condition was 0.042 ng ml{sup -1}. The extraction efficiency was investigated at different nickel concentrations (20-80 ng ml{sup -1}) and good recoveries (99.05-99.93%) were obtained using present method. The proposed method has been applied successfully for the determination of nickel in various water samples and compared with reported method in terms of Student's t-test and variance ratio f-test which indicate the significance of present method over reported and spectrophotometric methods at 95% confidence 0011lev.

  11. Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

    Institute of Scientific and Technical Information of China (English)

    Petr Lacina; Ludmila Mravcová; Milada Vávrová

    2013-01-01

    Pharmaceutical residues have become tightly controlled environmental contaminants in recent years,due to their increasing concentration in environmental components.This is mainly caused by their high level of production and everyday consumption.Therefore there is a need to apply new and sufficiently sensitive analytical methods,which can detect the presence of these contaminants even in very low concentrations.This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues,mainly from the group of non-steroidal anti-iaffammatory drugs (salicylic acid,acetylsalicylic acid,clofibric acid,ibuprofen,acetaminophen,caffeine,naproxen,mefenamic acid,ketoprofen,and dicofenac),in wastewaters and surface waters.This analytical method is based on solid phase extraction,derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GCxGC-TOF MS).Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix.The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice,Czech Republic.The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.

  12. HAB detection based on absorption and backscattering properties of phytoplankton

    Science.gov (United States)

    Lei, Hui; Pan, Delu; Bai, Yan; Chen, Xiaoyan; Zhou, Yan; Zhu, Qiankun

    2011-11-01

    The coastal area of East China Sea (ECS) suffers from the harmful algal blooms (HAB) frequently every year in the warm season. The most common causative phytoplankton algal species of HAB in the ECS in recent years are Prorocentrum donghaiense (dinoflagellates), Karenia mikimotoi (dinoflagellates which could produce hemolytic and ichthyotoxins) and Skeletonema costatum (diatom). The discrimination between the dinoflagellates and diatom HAB through ocean color remote sensing approach can add the knowledge of HAB events in ECS and help to the precaution. A series of in-situ measurement consisted of absorption coefficient, total scattering and particulate backscattering coefficient was conducted in the southern coast of Zhejiang Province in May 2009, and the estuary of Changjiang River in August 2009 and December 2010, which encountered two HAB events and a moderate bloom. The Inherent Optical Properties (IOPs) of the bloom waters have significant difference between phytoplankton species in absorption and backscattering properties. The chlorophyll a specific absorption coefficient (a*phy(λ)) for the bloom patches (chlorophyll a concentration >6mg m-3) differ greatly from the adjacent normal seawater, with the a*phy(λ) of bloom water lower than 0.03 m2 mg-1 while the a*phy(λ) of the adjacent normal seawater is much higher (even up to 0.06 m2 mg-1). Meanwhile, the backscattering coefficients at 6 wavebands (420, 442, 470, 510, 590 and 700nm) are also remarkably lower for bloom waters ( 0.02 m-1). The backscattering coefficient ratio (Rbp(λ)) is much lower for diatom bloom waters than for dinoflagellates types (0.01079 vs. 0.01227). A discrimination model based on IOPs is established, and several typical dinoflagellates and diatom bloom events including Prorocentrum donghaiense, Karenia mikimotoi and Skeletonema costatum in the ECS are picked out for testing with the MODIS-L2 and L3 ocean color remote sensing products from NASA website. The result proves that the

  13. Inventory of metal complexes circulating in plant fluids: a reliable method based on HPLC coupled with dual elemental and high-resolution molecular mass spectrometric detection.

    Science.gov (United States)

    Flis, Paulina; Ouerdane, Laurent; Grillet, Louis; Curie, Catherine; Mari, Stéphane; Lobinski, Ryszard

    2016-08-01

    Description of metal species in plant fluids such as xylem, phloem or related saps remains a complex challenge usually addressed either by liquid chromatography-mass spectrometry, X-ray analysis or computational prediction. To date, none of these techniques has achieved a complete and true picture of metal-containing species in plant fluids, especially for the least concentrated complexes. Here, we present a generic analytical methodology for a large-scale (> 10 metals, > 50 metal complexes) detection, identification and semiquantitative determination of metal complexes in the xylem and embryo sac liquid of the green pea, Pisum sativum. The procedure is based on direct injection using hydrophilic interaction chromatography with dual detection by elemental (inductively coupled plasma mass spectrometry) and molecular (high-resolution electrospray mass spectrometry) mass spectrometric detection. Numerous and novel complexes of iron(II), iron(III), copper(II), zinc, manganese, cobalt(II), cobalt(III), magnesium, calcium, nickel and molybdenum(IV) with several ligands including nicotianamine, citrate, malate, histidine, glutamine, aspartic acid, asparagine, phenylalanine and others are observed in pea fluids and discussed. This methodology provides a large inventory of various types of metal complexes, which is a significant asset for future biochemical and genetic studies into metal transport/homeostasis. PMID:27111838

  14. Environmental sample measurements with low background gamma-ray spectrometric systems

    Energy Technology Data Exchange (ETDEWEB)

    Tomarchio, E. [Palermo Univ., Dipt. di Ingegneria Nucleare Viale delle Scienze (Italy)

    2006-07-01

    This paper deals with the investigation of the performances of the spectrometric systems for measurement of environmental samples. The attention was focused on the determination of Minimum Detectable Activity for various geometries and, specifically, for air particulate samples collected on cellulose filters by an high-volume sampler (up to 20,000 m{sup 3}/day) and reduced to a square packet-sample geometry, 6 cm wide and 0.7 cm thick. A calibration procedure was experimented by adding a small amount of a radioactive powder to the sample matrix. In this way matrix self-absorption effects are intrinsically taken into account for each energy considered. Detection efficiency calibration was performed also for Marinelli beakers, well-suited for low-level activity measurement in large volume samples. The spectra detected on some environmental matrices have allowed evaluating very low activity concentration with a simple measurement technique, easily adoptable also in routine analyses.The spectrometric analyses performed on various environmental samples demonstrate the utility of low-level spectrometric systems, even situated at ground-level. The choice of a proper detector, with high radioactive purity and electronic components placed next the dewar, besides the selection of shielding materials, allows the determination of weak activity concentration with a good accuracy. The low detection limits reached with those spectrometric systems and the absence of significant photo peaks in the background spectra, detected for many days, allow the determination of activity concentration without incurring in complex stripping calculations of background photopeak components. Furthermore, efficiency calibration with the use of an homemade standard, previously calibrated by comparison with a commercial standard source, permits to take intrinsically into account self-absorption effects. At the present, L.E.P.S. (low energy photons spectrometer) is used to the daily determination of

  15. Identification of Polish cochineal (Porphyrophora polonica L.) in historical textiles by high-performance liquid chromatography coupled with spectrophotometric and tandem mass spectrometric detection.

    Science.gov (United States)

    Lech, Katarzyna; Jarosz, Maciej

    2016-05-01

    The present work reports a method for identification of Polish cochineal (Porphyrophora polonica L.) in historical fabrics by the use of high-performance liquid chromatography coupled with diode array and tandem mass spectrometric detection with electrospray ionization (HPLC-DAD-ESI MS/MS). This hyphened technique allows detection and identification of 16 new minor colorants present in the discussed scale insect (including two previously observed by Wouters and Verhecken (Ann Soc Entomol Fr. 1989;25:393-410), but specified only as compounds of unknown structures) that do not occur (e.g., in American cochineal). The MS/MS experiments, complemented with UV-VIS data, enable identification of mono- and di-, C- and O-hexosides of kermesic and flavokermesic acids or their derivatives. The present paper introduces a fingerprint of color compounds present in Polish cochineal and defines them, particularly pp6 (ppI, O-hexoside of flavokermesic acid), as its markers allow distinguishing of Polish-cochineal reds from the American ones. Usefulness of the selected set of markers for identification of Polish cochineal has been demonstrated in the examination of textiles from the collection of the National Museum in Warsaw using the multiple reaction monitoring (MRM) method, originally elaborated on the basis of this study. PMID:26935929

  16. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Steffen, S. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Otto, M. [TU Bergakademie Freiberg (TU BAF), Institute for Analytical Chemistry, Leipziger Str. 29, D - 09599 Freiberg (Germany)], E-mail: matthias.otto@chemie.tu-freiberg.de; Niewoehner, L.; Barth, M. [Bundeskriminalamt (BKA), Forensic Science Institute KT23, Thaerstr. 11, D - 65193 Wiesbaden (Germany); Brozek-Mucha, Z. [Instytut Ekspertyz Sadowych (IES), Westerplatte St. 9, PL - 31-033 Krakow (Poland); Biegstraaten, J. [Nederlands Forensisch Instituut (NFI), Fysische Technologie, Laan van Ypenburg 6, NL-2497 GB Den Haag (Netherlands); Horvath, R. [Kriminalisticky a Expertizny Ustav (KEU PZ), Institute of Forensic Science, Sklabinska 1, SK - 812 72 Bratislava (Slovakia)

    2007-09-15

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

  17. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    International Nuclear Information System (INIS)

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification

  18. A method of test for residual isophorone diisocyanate trimer in new polyester-polyurethane coatings on light metal packaging using liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Driffield, Malcolm; Bradley, Emma L; Castle, Laurence

    2007-02-01

    A method of test for residual isophorone diisocyanate (IPDI) trimer in experimental formulation polyester-polyurethane (PEPU) thermoset coatings on metal food packaging is described. The method involves extraction of coated panels using acetonitrile containing dibutylamine for concurrent derivatisation, and then high performance liquid chromatography with electrospray ionisation tandem mass spectrometric detection (LC-MS/MS). Single laboratory validation was carried out using three different experimental PEPU-based coatings. The calibrations were linear, the analytical recovery was good, no interferences were seen, and substance identification criteria were met. The detection limit of the method is around 0.02 micro g/100 cm(2) of coating, which for a typical sized can and assuming complete migration of any residual IPDI trimer, corresponds to about 0.2 micro g/kg food or beverage. Separate studies indicated that, even if migration occurred at such low levels, the IPDI trimer would not be expected to persist in canned aqueous or fatty foodstuffs as it would hydrolyse to the corresponding aliphatic amine or react with food components to destroy the isocyanate moiety. The method of test developed here for residual IPDI trimer in thermoset polyester-polyurethane coatings should prove to be a valuable tool for investigating the cure kinetics of these novel coatings and help to guide the development of enhanced formulations.

  19. A method of test for residual isophorone diisocyanate trimer in new polyester-polyurethane coatings on light metal packaging using liquid chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Driffield, Malcolm; Bradley, Emma L; Castle, Laurence

    2007-02-01

    A method of test for residual isophorone diisocyanate (IPDI) trimer in experimental formulation polyester-polyurethane (PEPU) thermoset coatings on metal food packaging is described. The method involves extraction of coated panels using acetonitrile containing dibutylamine for concurrent derivatisation, and then high performance liquid chromatography with electrospray ionisation tandem mass spectrometric detection (LC-MS/MS). Single laboratory validation was carried out using three different experimental PEPU-based coatings. The calibrations were linear, the analytical recovery was good, no interferences were seen, and substance identification criteria were met. The detection limit of the method is around 0.02 micro g/100 cm(2) of coating, which for a typical sized can and assuming complete migration of any residual IPDI trimer, corresponds to about 0.2 micro g/kg food or beverage. Separate studies indicated that, even if migration occurred at such low levels, the IPDI trimer would not be expected to persist in canned aqueous or fatty foodstuffs as it would hydrolyse to the corresponding aliphatic amine or react with food components to destroy the isocyanate moiety. The method of test developed here for residual IPDI trimer in thermoset polyester-polyurethane coatings should prove to be a valuable tool for investigating the cure kinetics of these novel coatings and help to guide the development of enhanced formulations. PMID:17178416

  20. Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

    Science.gov (United States)

    Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Bro¿żek-Mucha, Z.; Biegstraaten, J.; Horváth, R.

    2007-09-01

    A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

  1. Spectrometric techniques 4

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  2. Atomic-absorption spectrometric, neutron-activation and radioanalytical techniques for the determination of trace metals in environmental, biochemical and toxicological research

    International Nuclear Information System (INIS)

    Radioanalytical techniques and atomic-absorption spectrometry have been used for the micro-determination of vanadium in biological specimens such as human tissues and body fluids in environmental, biochemical and toxicological research. The use of 48V as a radiotracer permitted investigations on the vaporisation and retention mechanisms of vanadium. Higher vanadium oxides are probably converted into lower oxides, decomposing to VO in gaseous form, followed by the dissociation to 'free vanadium' and oxygen. It was found that about 20% of the 48V radioactivity was consistently retained in the graphite tube after 10 repeated introductions and firings of 50 μl of 50 ng ml-148V-labelled vanadium solution. However, the amount retained, probably in the form of carbide, does not vaporise under the conditions used for the analysis. Determinations of vanadium at the parts per billion level in 10 urine samples by neutron-activation analysis and by graphite furnace atomic-absorption spectrometry showed agreement that can be considered satisfactory for practical purposes. (author)

  3. Valence-to-core-detected X-ray absorption spectroscopy

    DEFF Research Database (Denmark)

    Hall, Eleanor R.; Pollock, Christopher J.; Bendix, Jesper;

    2014-01-01

    X-ray absorption spectroscopy (XAS) can provide detailed insight into the electronic and geometric structures of transition-metal active sites in metalloproteins and chemical catalysts. However, standard XAS spectra inherently represent an average contribution from the entire coordination...

  4. Validation of method for determination of different classes of pesticides in aqueous samples by dispersive liquid-liquid microextraction with liquid chromatography-tandem mass spectrometric detection.

    Science.gov (United States)

    Caldas, Sergiane Souza; Costa, Fabiane Pinho; Primel, Ednei Gilberto

    2010-04-14

    In this study, a simple, rapid and efficient method has been developed for the extraction and preconcentration of different classes of pesticides, carbofuran (insecticide), clomazone (herbicide) and tebuconazole (fungicide) in aqueous samples by dispersive liquid-liquid microextraction (DLLME) coupled with liquid chromatography-tandem mass spectrometric detection. Some experimental parameters that influence the extraction efficiency, such as the type and volume of the disperser solvents and extraction solvents, extraction time, speed of centrifugation, pH and addition of salt were examined and optimized. Under the optimum conditions, the recoveries of pesticides in water at spiking levels between 0.02 and 2.0 microg L(-1) ranged from 62.7% to 120.0%. The relative standard deviations varied between 1.9% and 9.1% (n=3). The limits of quantification of the method considering a 50-fold preconcentration step were 0.02 microg L(-1). The linearity of the method ranged from 1.0 to 1000 microg L(-1) for all compounds, with correlation coefficients varying from 0.9982 to 0.9992. Results show that the method we propose can meet the requirements for the determination of pesticides in water samples. The comparison of this method with solid-phase extraction indicates that DLLME is a simple, fast, and low-cost method for the determination of pesticides in natural waters.

  5. Preconcentration and atomic absorption spectrometric determination of cadmium, cobalt, copper, iron, lead, manganese, nickel and zinc in water samples using 6-methyl-2-pyridinecarboxaldehyde-4-phenyl-3-thiosemicarbazone

    International Nuclear Information System (INIS)

    The reagent 6-methyl-2-pyridinecarboxaldehyde-4-phenyl-3-thiosemicarbazone (MPAPT) has been examined for the pre-concentration of metal ions and determination using air acetylene flame atomic absorption spectrometer. The method is based on the complexation and extraction of cadmium (II), cobalt(III), copper(II), lead(II), nickel(II), iron(II), iron(II), manganese(II) and zinc(II) in chloroform. The metal iron are back extracted in nitric acid (1:1) or after evaporation of solvent the residue is digested in nitric acid. After necessary adjustment of volume the metal ions were determined in aqueous solution. Pre-concentration is obtained 10-25 times. Metal ions recovery was 95.4-100.8% with coefficient of variation 0.2-7.5%. The method used for the determination of metals in canal and sewerage waters, within 2-6433 mu g/L with C. V 0.-5.2%. (author)

  6. Sensitive detection of tunable diode laser absorption by polarization rotation

    International Nuclear Information System (INIS)

    Results are presented demonstrating that diode laser absorption sensitivity can be increased by using the Faraday or Kerr effect to rotate the polarization of the source so that crossed polarizers can be used to reduce source noise. The Faraday effect is demonstrated using nitric oxide in a magnetic field, and the Kerr effect is demonstrated using methyl fluoride in an electric field. Some description of how absorption in an external field causes polarization rotation is presented as well as some conclusions on the types of molecules for which this technique is best suited

  7. Flame atomic absorption spectrometric determination of trace amounts of heavy metal ions after solid phase extraction using modified sodium dodecyl sulfate coated on alumina

    International Nuclear Information System (INIS)

    A sensitive and selective solid phase extraction procedure for the determination of traces of Cu(II), Zn(II), Pb(II) and Fe(III) has been developed. An alumina-sodium dodecyl sulfate (SDS) coated on with meso-phenyl bis(indolyl) methane (MPBIM) was used for preconcentration and determination of Cu(II), Zn(II), Pb(II) and Fe(III) ions by flame atomic absorption spectrometry. The analyte ions were adsorbed quantitatively on adsorbent due to their complexation with MPBIM. Adsorbed metals were quantitatively eluted using 6 mL of 4 mol L-1 nitric acid. The effects of parameters such as pH, amount of alumina, amount of MBITP, flow rate, type and concentration of eluting agent were examined. The effects of interfering ions on the separation-preconcentration of analytes were also investigated. The relative standard deviation of the method was found to be less than 3.0%. The presented procedure was successfully applied for determination of analytes in real samples

  8. Determination of calcium, magnesium, sodium, and potassium in foodstuffs by using a microsampling flame atomic absorption spectrometric method after closed-vessel microwave digestion: method validation.

    Science.gov (United States)

    Chekri, Rachida; Noël, Laurent; Vastel, Christelle; Millour, Sandrine; Kadar, Ali; Guérin, Thierry

    2010-01-01

    This paper describes a validation process in compliance with the NFIEN ISO/IEC 17025 standard for the determination of the macrominerals calcium, magnesium, sodium, and potassium in foodstuffs by microsampling with flame atomic absorption spectrometry after closed-vessel microwave digestion. The French Standards Commission (Agence Francaise de Normalisation) standards NF V03-110, NF EN V03-115, and XP T-90-210 were used to evaluate this method. The method was validated in the context of an analysis of the 1322 food samples of the second French Total Diet Study (TDS). Several performance criteria (linearity, LOQ, specificity, trueness, precision under repeatability conditions, and intermediate precision reproducibility) were evaluated. Furthermore, the method was monitored by several internal quality controls. The LOQ values obtained (25, 5, 8.3, and 8.3 mg/kg for Ca, Mg, Na, and K, respectively) were in compliance with the needs of the TDS. The method provided accurate results as demonstrated by a repeatability CV (CVr) of < 7% and a reproducibility CV (CVR) of < 12% for all the elements. Therefore, the results indicated that this method could be used in the laboratory for the routine determination of these four elements in foodstuffs with acceptable analytical performance. PMID:21313817

  9. Application of high-performance liquid chromatography combined with ultra-sensitive thermal lens spectrometric detection for simultaneous biliverdin and bilirubin assessment at trace levels in human serum.

    Science.gov (United States)

    Martelanc, Mitja; Žiberna, Lovro; Passamonti, Sabina; Franko, Mladen

    2016-07-01

    We present the applicability of a new ultra-sensitive analytical method for the simultaneous determination of biliverdin and bilirubin in human serum. The method comprises isocratic reversed-phase (RP) C18 high-performance liquid chromatography (HPLC) and thermal lens spectrometric detection (TLS) based on excitation by a krypton laser emission line at 407nm. This method enables the separation of IX-α biliverdin and IX-α bilirubin in 11min with limit of detection (LOD) and limit of quantitation (LOQ) for biliverdin of 1.2nM and 3nM, and 1nM and 2.8nM for bilirubin, respectively. In addition, a step-gradient elution was set up, by changing the mobile phase composition, in order to further enhance the sensitivity for bilirubin determination with LOD and LOQ of 0.5nM and 1.5nM, respectively. In parallel, an isocratic HPLC-DAD method was developed for benchmarking against HPLC-TLS methods. The LOD and LOQ for biliverdin were 6nM and 18nM, and 2.5nM and 8nM for bilirubin, respectively. Additionally, both isocratic methods were applied for measuring biliverdin and free bilirubin in human serum samples (from 2 male and 2 female healthy donors). Combining isocratic HPLC method with TLS detector was crucial for first ever biliverdin determination in serum together with simultaneous free bilirubin determination. We showed for the first time the concentration ratio of free bilirubin versus unbound biliverdin in human serum samples. PMID:27154653

  10. A multiresidue liquid chromatographic/tandem mass spectrometric method for the detection and quantitation of 15 nonsteroidal anti-inflammatory drugs (NSAIDs) in bovine meat and milk.

    Science.gov (United States)

    van Pamel, Els; Daeseleire, Els

    2015-06-01

    This study concerns a validated liquid chromatographic/tandem mass spectrometric (LC-MS/MS) multiresidue method for the simultaneous detection, identification, and quantitation of 15 nonsteroidal anti-inflammatory drugs (NSAIDs) in bovine meat and milk. The NSAIDs considered are carprofen, diclofenac, flufenamic acid, flunixin (5-hydroxyflunixin as marker metabolite in milk), ketoprofen, mefenamic acid, meloxicam, 4-methylaminoantipyrine (marker metabolite of metamizole in meat and milk), naproxen, niflumic acid, phenylbutazone (and metabolite oxyphenbutazone), ramifenazone, salicylic acid, and tolfenamic acid. These compounds were chosen as representatives of different chemical subclasses of NSAIDs. Flunixin-d3, diclofenac-d4, 4-aminoantipyrine-d3, and phenylbutazone-d10 were used as internal standards. Performance characteristics were validated according to the Commission Decision 2002/657/EC (Off J Eur Communities, L221: 8-36). Recovery percentages varied between 81 and 114% for bovine meat and between 79 and 118% for milk. Repeatability percentages were within the range of 1-12% for meat and between 1 and 17% for milk, whereas the intralaboratory reproducibility varied between 3 and 19% for meat and between 3 and 23% for milk. The decision limit and the detection capability for bovine meat were within the range of 0.5-579 μg kg(-1)and 0.6-642 μg kg(-1), respectively. Those for milk were within the range of 0.12-55 μg kg(-1) and 0.14-61 μg kg(-1), respectively. The methods developed were successfully applied for proficiency test samples and routine samples analyzed in the laboratory. The methodology concerns fast, user-friendly, and sensitive methods, which can be easily extended for other compounds and matrices. In general, such multiresidue methods contribute to the reduction of human exposure to these veterinary drug residues by consumption of contaminated bovine-derived products such as meat and milk.

  11. Ultrasensitive molecular absorption detection using metal slot antenna arrays.

    Science.gov (United States)

    Ahn, Kwang Jun; Bahk, Young-Mi; Kim, Dai-Sik; Kyoung, Jisoo; Rotermund, Fabian

    2015-07-27

    We theoretically study the transmission reduction of light passing through absorptive molecules embedded in a periodic metal slot array in a near infrared wavelength regime. From the analytically solved transmitted light, we present a simple relation given by the attenuation length of light at the resonance wavelength of the slot antennas with respect to the spectral width of the resonant transmission peak. This relation clearly explains that the control of the transmission reduction even with very low absorptive materials is possible. We investigate also the transmission reduction by absorptive molecules in a real metallic slot antenna array on a dielectric substrate and compare the results with finite difference time domain calculations. In numerical calculations, we demonstrate that the same amount of transmission reduction by a bulk absorptive material can be achieved only with one-hundredth thickness of the same material when it is embedded in an optimized Fano-resonant slot antenna array. Our relation presented in this study can contribute to label-free chemical and biological sensing as an efficient design and performance criterion for periodic slot antenna arrays. PMID:26367567

  12. On-line two-dimensional capillary electrophoresis with mass spectrometric detection using a fully electric isolated mechanical valve.

    Science.gov (United States)

    Kohl, Felix J; Montealegre, Cristina; Neusüß, Christian

    2016-04-01

    CE is becoming more and more important in many fields of bioanalytical chemistry. Besides optical detection, hyphenation to ESI-MS detection is increasingly applied for sensitive identification purposes. Unfortunately, many CE techniques and methods established in research and industry are not compatible to ESI-MS since essential components of the background electrolyte interfere in ES ionization. In order to identify unknown peaks in established CE methods, here, a heart-cut 2D-CE separation system is introduced using a fully isolated mechanical valve with an internal loop of only 20 nL. In this system, the sample is separated using potentially any non-ESI compatible method in the first separation dimension. Subsequently, the portion of interest is cut by the internal sample loop of the valve and reintroduced to the second dimension where the interfering compounds are removed, followed by ESI-MS detection. When comparing the separation efficiency of the system with the valve to a system using a continuous capillary only a slight increase in peak width is observed. Ultraviolet/visible detection is integrated in the first dimension for switching time determination, enabling reproducible cutting of peaks of interest. The feasibility of the system is successfully demonstrated by a 2D analysis of a BSA tryptic digest sample using a nonvolatile (phosphate based) background electrolyte in the first dimension.

  13. Flame Atomic Absorption Spectrometric Determination of Gold After Solid-Phase Extraction of Its 2-Aminobenzothiazole Complex on Diaion SP-207.

    Science.gov (United States)

    Unsal, Yunus Emre; Tuzen, Mustafa; Soylak, Mustafa

    2016-03-01

    An SPE of Au (III) on a 2-aminobenzothiazole-coated Diaion SP 207-column system has been developed. The parameters, including pH of solution, amount of 2-aminobenzothiazole, eluent type, sample volume, and flow rates, were examined. The effects of alkali, alkali earth, and some metals were also studied. The recovery values at optimal conditions and detection limits for Au (III) were found as >95% and 3.8 μg L(-1), respectively. The factor of preconcentration was 250. The RSD value was determination of gold was applied to water, mine, soil, and anodic slime samples. PMID:26964845

  14. A mid-infrared absorption diagnostic for acetylene detection

    KAUST Repository

    KC, Utsav

    2015-05-14

    Acetylene is an important combustion intermediate and plays a critical role in soot formation. Accurate measurements of trace concentrations of acetylene can be very useful in validating hydrocarbon oxidation and soot formation mechanisms. Strongest vibrational band of acetylene near 13.7 μm is probed here to develop a highly sensitive absorption diagnostic. Experiments are carried out behind reflected shock waves to measure absorption cross sections of acetylene near 730 cm−1 over a wide range of temperatures (1000–2200 K) and pressures (1–5 bar). The diagnostic is demonstrated by measuring acetylene formation during the shock-heated pyrolysis and oxidation of propene. © 2015 Springer-Verlag Berlin Heidelberg

  15. Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations

    International Nuclear Information System (INIS)

    A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 μg/l for iron-3.4 μg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey

  16. Spectrometric techniques 3

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume III presents the applications of spectrometric techniques to atmospheric and space studies. This book reviews the spectral data processing and analysis techniques that are of broad applicability.Organized into five chapters, this volume begins with an overview of the instrumentation used for obtaining field data. This text then reviews the contribution that space-borne spectroscopy in the thermal IR has made to the understanding of the planets. Other chapters consider the instruments that have recorded the planetary emission spectra. This book discusses as well

  17. A new preconcentration and separation method for flame atomic absorption spectrometric determinations of some trace metal ions on a diaion HP-20 column

    International Nuclear Information System (INIS)

    A preconcentration/separation method for determination of Cr(3), Cd(2), Bi(3) and Co(2) has been proposed. The analytes were adsorbed on a column filled Diaion HP-20 resin as metal-8-hydroxiquinoline complexes and desorbed from the column by using 10 ml of 1M HNO3 in acetone. The influences of some analytical parameters such as pH, amounts of oxine, type of eluent etc on the recoveries of chromium, cadmium, bismuth and cobalt were discussed. Effects of the various alkaline salts on the recoveries of the investigated ions were also examined. The method was applied for the determination of Cr(3), Cd(2), Bi(3), and Co(2) contents of table salt samples, some chemical grade alkaline salts produced in Turkey and a stream sediment standard reference material sample (GBW 07309) with satisfactory results (recoveries > 95%, relative standard deviations < 9%). The limit of detection for analyte ions (3s, N=20) was between 23-305 ng/g

  18. Determination of free amino compounds in betalainic fruits and vegetables by gas chromatography with flame ionization and mass spectrometric detection.

    Science.gov (United States)

    Kugler, Florian; Graneis, Stephan; Schreiter, Pat P-Y; Stintzing, Florian C; Carle, Reinhold

    2006-06-14

    Amino acids and amines are the precursors of betalains. Therefore, the profiles of free amino compounds in juices obtained from cactus pears [Opuntia ficus-indica (L.) Mill. cv. Bianca, cv. Gialla, and cv. Rossa], pitaya fruits [Selenicereus megalanthus (K. Schumann ex Vaupel) Moran, Hylocereus polyrhizus (Weber) Britton & Rose, and Hylocereus undatus (Haworth) Britton & Rose], and in extracts from differently colored Swiss chard [Beta vulgaris L. ssp. cicla (L.) Alef. cv. Bright Lights] petioles and red and yellow beets (B. vulgaris L. ssp. vulgaris var. conditiva Alef. cv. Burpee's Golden) were investigated for the first time. Amino compounds were derivatized with propyl chloroformate. While gas chromatography (GC) with mass spectrometry was used for peak assignment, GC flame ionization detection was applied for quantification of individual compounds. Whereas proline was the major free amino compound of cactus pear and pitaya fruit juices, glutamine dominated in Swiss chard stems and beets, respectively. Interestingly, extremely high concentrations of dopamine were detected in Swiss chard stems and beets. Furthermore, the cleavage of betaxanthins caused by derivatization in alkaline reaction solutions is demonstrated for the first time. Amino acids and amines thus released might increase the actual free amino compound contents of the respective sample. To evaluate the contribution of betaxanthin cleavage to total amino acid and amine concentration, isolated betaxanthins were derivatized according to the "EZ:faast" method prior to quantification of the respective amino compounds released. On a molar basis, betaxanthin contribution to overall amino compound contents was always below 6.4%. PMID:16756361

  19. Prototype explosives detection system based on nuclear resonance absorption in nitrogen

    Energy Technology Data Exchange (ETDEWEB)

    Morgado, R.E.; Arnone, G.; Cappiello, C.C.; Gardner, S.D.; Hollas, C.L.; Ussery, L.E.; White, J.M.; Zahrt, J.D. [Los Alamos National Lab., NM (United States); Krauss, R.A. [Federal Aviation Administration, Atlantic City, NJ (United States)

    1993-12-01

    A-prototype explosives detection system that was developed for experimental evaluation of a nuclear resonance absorption techniques is described. The major subsystems are a proton accelerator and beam transport, high-temperature proton target, an airline-luggage tomographic inspection station, and an image-processing/detection- alarm subsystem. The detection system performance, based on a limited experimental test, is reported.

  20. Flame atomic absorption spectrometric (FAAS) determination of copper, iron and zinc in food samples after solid-phase extraction on Schiff base-modified duolite XAD 761

    International Nuclear Information System (INIS)

    The present study involves the development of solid-phase extraction (SPE) procedure for the preconcentration of trace amounts of copper (Cu2+), iron (Fe3+) and zinc (Zn2+) ions on duolite XAD 761 modified by bis(2-hydroxyacetophenone)-2,2-dimethyl-1,3-propanediimine(BHAPDMPDI). The complexation between the metal ions and the proposed ligand was investigated potentiometrically. The metal ions retained on the sorbent were quantitatively determined via complexation with BHAPDMPDI. The complexed metal ions were efficiently eluted using 6 mL of 4 mol L−1 nitric acid in acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ions were optimized. Using the optimized parameters, the linear response of the SPE method for Cu2+, Zn2+ and Fe3+ ions were in the ranges of 0.01–0.34, 0.01–0.28 and 0.02–0.31 μg mL−1, respectively, and the detection limits for Cu2+, Zn2+ and Fe3+ ions were 1.8, 1.6 and 2.4 μg mL−1, respectively. The proposed method exhibits a preconcentration factor of 208 for all of the ions studied and an enhancement factor for Cu2+, Fe3+ and Zn2+ ions of 34, 28 and 38, respectively. The presented results demonstrate the successful application of the proposed method for the determination of these metal ions in some real samples with high recoveries (> 95%) and reasonable relative standard deviation (RDS < 5%). Highlights: ► Highly efficient adsorbent for dye removal was synthesized. ► The sorbent was fully characterized. ► The proposed method has a potential of a waste water treatment alternative. ► Excellent properties of the sorbent have been illustrated in detail

  1. Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection.

    Science.gov (United States)

    Zygler, Agata; Wasik, Andrzej; Kot-Wasik, Agata; Namieśnik, Jacek

    2011-06-01

    An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame (ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC) and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer composed of formic acid and N,N-diisopropylethylamine at pH 4.5 in ultrasonic bath, extracts were cleaned up using Strata-X 33 μm Polymeric SPE column. The analytes were separated in gradient elution mode on C(18) column and detected by mass spectrometer working with an electrospray source in negative ion mode. To confirm that analytical method is suitable for its intended use, several validation parameters, such as linearity, limits of detection and quantification, trueness and repeatibilty were evaluated. Calibration curves were linear within a studied range of concentrations (r(2) ≥ 0.999) for six investigated sweeteners (CYC, ASP, ALI, DUL, NHDC, NEO). Three compounds (ACS-K, SAC, SCL) gave non-linear response in the investigated concentration range. The method detection limits (corresponding to signal-to-noise (S/N) ratio of 3) were below 0.25 μg mL(-1) (μg g(-1)), whereas the method quantitation limits (corresponding to S/N ratio of 10) were below 2.5 μg mL(-1) (μg g(-1)). The recoveries at the tested concentrations (50%, 100% and 125% of maximum usable dose) for all sweeteners were in the range of 84.2 ÷ 106.7%, with relative standard deviations sweeteners in drinks, yoghurts and fish products. The procedure described here is simple, accurate and precise and is suitable for routine quality control analysis of foodstuffs. PMID:21465096

  2. Filtering absorption and visual detection of methylene blue by nitrated cellulose acetate membrane

    Energy Technology Data Exchange (ETDEWEB)

    He, Shengbin; Fang, He; Xu, Xiaoping [College of Chemistry, Fuzhou University, Fuzhou (China)

    2016-04-15

    Wastewater-containing industrial dyes are quite harmful since most dyes are stable and toxic to humans. Detection and removing of those dyes from wastewater is necessary to ensure water supply safety. In present work, a nitrated cellulose acetate (NCA) microfiltration membrane was developed for specific absorption and visible detection of methylene blue (MB). The NCA microfiltration membrane overcomes the defect of high driven pressure in nanofiltration or ultrafiltration process. By absorption effect, the NCA membrane also overcomes the defect of low retention rate of traditional microfiltration membrane to dyes. The residual MB can be removed quickly and thoroughly by microfiltration absorption. The microfiltration membrane can also be used for visual detection of MB by concentrating the MB on membrane. The limit of detection is as low as 0.001 mg/L. The detection method is simple and free of large-scale instrument, and can be used as a portable device for spot detection of dye-contaminated water.

  3. Matrix isolation Fourier transform infrared spectrometric detection in the open tubular column gas chromatography of polycyclic aromatic hydrocarbons

    Energy Technology Data Exchange (ETDEWEB)

    Hembree, D.M.; Garrison, A.A.; Crocombe, R.A.; Yokley, R.A.; Wehry, E.L.; Mamantov, G.

    1981-10-01

    A detailed description of a system for gas chromatographic (GC) detection of matrix isolation Fourier transform infrared (FTIR) spectrometry is presented. Substances eluting from a support-coated open tubular column are deposited directly on individual faces of a 12-sided movable gold-plated copper disk mounted within the cold head of a closed-cycle cryostat. The same gas is used as GC carrier and spectroscopic matrix gas. An optical interface, comprising beam condensing and rod optics, permits the modified cryostat head to be mounted in proximity to the sample chamber of an FTIR spectrometer. Applications of the technique to identification of polycyclic aromatic hydrocarbon constituents of coal-derived materials are demonstrated, and quantitative aspects of the procedure are considered.

  4. Determination of plasticizers included in balloon by solid phase microextraction and gas chromatography with mass spectrometric detection.

    Energy Technology Data Exchange (ETDEWEB)

    Park, H.M.; Kim, J.H.; Ryu, J.Ch.; Kim, Y.M.; Lee, K.B. [Korea Institute of Science and Technology, Seoul (Korea)

    2001-02-01

    Solid-phase microextraction (SPME) with 85 {mu}m polyacrylate fiber, coupled to gas chromatography-mass spectrometry was used to analyze the plasticizers contained in balloon samples. The balloons were identified to be made of polyisoprene by IR spectroscopy. The plasticizers extracted from the balloon samples soaked in acetone-added water solvent for an hour were quantified by external standard method using nine kinds of plasticizers. The quantification method was validated for standard plasticizers in the range of 0.25-25 {mu}g/g. The detection limits were 0.11-0.38 {mu}g/g for different plasticizers. The RSDs for the reproducibility of this quantitation method were 3.7-14.2%. A few of balloons included risky level of plasticizer concerned as an endocrine disrupter, and it is necessary to regulate these products. (author). 10 refs., 3 tabs., 4 figs.

  5. Detection of drugs in lifted cyanoacrylate-developed latent fingermarks using two laser desorption/ionisation mass spectrometric methods.

    Science.gov (United States)

    Sundar, Latha; Rowell, Frederick

    2014-02-01

    This paper describes a method for lifting cyanoacrylate (CNA)-developed latent fingermarks from a glass surface and the detection of five drugs in lifted marks from fingers that had been in contact with the drugs, using Surface Assisted Laser Desorption Ionisation Time of Flight Mass Spectrometry (SALDI-TOF-MS) or Matrix Assisted Laser Desorption Ionisation TOF-MS (MALDI-TOF-MS). Two drugs of abuse (cocaine and methadone) and three therapeutic drugs (aspirin, paracetamol and caffeine) were used as contact residues. Latent fingermarks spiked with the drugs were subjected to CNA fuming followed by dusting with ARRO SupraNano™ MS black magnetic powder (SALDI-TOF-MS) or 2,5-dihydroxybenzoic acid (DHB) (MALDI-TOF-MS). The dusted mark was then exposed to solvent vapour before lifting with a commercial fingerprint lifting tape following established procedures. The presence of the drugs was then confirmed by direct analysis on the tape without further processing using SALDI- or MALDI-TOF-MS. The black magnetic fingerprint powder provided visual enhancement of the CNA-fingermark while no visual enhancement was observed for marks dusted with DHB powder. Similar [M + H](+) peaks for all the drug analytes were observed for both methods along with some sodium and potassium adducts for SALDI-MS and some major fragment ions but the SALDI signals were generally more intense. Simple exposure to acetone vapour of the CNA-developed marks enabled their effective transfer onto the tape which was crucial for subsequent MS detection of the analytes.

  6. Determination and characterization of phytochelatins by liquid chromatography coupled with on line chemical vapour generation and atomic fluorescence spectrometric detection.

    Science.gov (United States)

    Bramanti, Emilia; Toncelli, Daniel; Morelli, Elisabetta; Lampugnani, Leonardo; Zamboni, Roberto; Miller, Keith E; Zemetra, Joseph; D'Ulivo, Alessandro

    2006-11-10

    Liquid chromatography (LC) coupled on line with UV/visible diode array detector (DAD) and cold vapour generation atomic fluorescence spectrometry (CVGAFS) has been developed for the speciation, determination and characterization of phytochelatins (PCs). The method is based on a bidimensional approach, e.g. on the analysis of synthetic PC solutions (apo-PCs and Cd(2+)-complexed PCs) (i) by size exclusion chromatography coupled to UV diode array detector (SEC-DAD); (ii) by the derivatization of PC -SH groups in SEC fractions by p-hydroxymercurybenzoate (PHMB) and the indirect detection of PC-PHMB complexes by reversed phase liquid chromatography coupled to atomic fluorescence detector (RPLC-CVGAFS). MALDI-TOF/MS (matrix assisted laser desorption ionization time of flight mass spectrometry) analysis of underivatized synthetic PC samples was performed in order have a qualitative information of their composition. Quantitative analysis of synthetic PC solutions has been performed on the basis of peak area of PC-PHMB complexes of the mercury specific chromatogram and calibration curve of standard solution of glutathione (GSH) complexed to PHMB (GS-PHMB). The limit of quantitation (LOQ) in terms of GS-PHMB complex was 90 nM (CV 5%) with an injection volume of 35 microL, corresponding to 3.2 pmol (0.97 ng) of GSH. The method has been applied to analysis of extracts of cell cultures from Phaeodactylum tricornutum grown in Cd-containing nutrient solutions, analysed by SEC-DAD-CVGAFS and RPLC-DAD-CVGAFS.

  7. Airborne Measurements of CO2 Column Absorption and Range Using a Pulsed Direct-Detection Integrated Path Differential Absorption Lidar

    Science.gov (United States)

    Abshire, James B.; Riris, Haris; Weaver, Clark J.; Mao, Jianping; Allan, Graham R.; Hasselbrack, William E.; Browell, Edward V.

    2013-01-01

    We report on airborne CO2 column absorption measurements made in 2009 with a pulsed direct-detection lidar operating at 1572.33 nm and utilizing the integrated path differential absorption technique. We demonstrated these at different altitudes from an aircraft in July and August in flights over four locations in the central and eastern United States. The results show clear CO2 line shape and absorption signals, which follow the expected changes with aircraft altitude from 3 to 13 km. The lidar measurement statistics were also calculated for each flight as a function of altitude. The optical depth varied nearly linearly with altitude, consistent with calculations based on atmospheric models. The scatter in the optical depth measurements varied with aircraft altitude as expected, and the median measurement precisions for the column varied from 0.9 to 1.2 ppm. The altitude range with the lowest scatter was 810 km, and the majority of measurements for the column within it had precisions between 0.2 and 0.9 ppm.

  8. Probing the dynamics of polyatomic multichannel elementary reactions by crossed molecular beam experiments with soft electron-ionization mass spectrometric detection.

    Science.gov (United States)

    Casavecchia, Piergiorgio; Leonori, Francesca; Balucani, Nadia; Petrucci, Raffaele; Capozza, Giovanni; Segoloni, Enrico

    2009-01-01

    In this Perspective we highlight developments in the field of chemical reaction dynamics. Focus is on the advances recently made in the investigation of the dynamics of elementary multichannel radical-molecule and radical-radical reactions, as they have become possible using an improved crossed molecular beam scattering apparatus with universal electron-ionization mass spectrometric detection and time-of-flight analysis. These improvements consist in the implementation of (a) soft ionization detection by tunable low-energy electrons which has permitted us to reduce interfering signals originating from dissociative ionization processes, usually representing a major complication, (b) different beam crossing-angle set-ups which have permitted us to extend the range of collision energies over which a reaction can be studied, from very low (a few kJ mol(-1), as of interest in astrochemistry or planetary atmospheric chemistry) to quite high energies (several tens of kJ mol(-1), as of interest in high temperature combustion systems), and (c) continuous supersonic sources for producing a wide variety of atomic and molecular radical reactant beams. Exploiting these new features it has become possible to tackle the dynamics of a variety of polyatomic multichannel reactions, such as those occurring in many environments ranging from combustion and plasmas to terrestrial/planetary atmospheres and interstellar clouds. By measuring product angular and velocity distributions, after having suppressed or mitigated, when needed, the problem of dissociative ionization of interfering species (reactants, products, background gases) by soft ionization detection, essentially all primary reaction products can be identified, the dynamics of each reaction channel characterized, and the branching ratios determined as a function of collision energy. In general this information, besides being of fundamental relevance, is required for a predictive description of the chemistry of these

  9. An absorption detection approach for multiplexed capillary electrophoresis using a linear photodiode array.

    Science.gov (United States)

    Gong, X; Yeung, E S

    1999-11-01

    A novel absorption detection method for highly multiplexed capillary electrophoresis is presented for zone electrophoresis and for micellar electrokinetic chromatography. The approach involves the use of a linear photodiode array on which a capillary array is imaged by a camera lens. Either a tungsten lamp or a mercury lamp can be used as the light source such that all common wavelengths for absorption detection are accessible by simply interchanging narrow-band filters. Each capillary spans several diodes in the photodiode array for absorption measurements. Over 100 densely packed capillaries can be monitored by a single photodiode array element with 1024 diodes. The detection limit for rhodamine 6G for each capillary in the multiplexed array is ∼1.8 × 10(-)(8) M injected (S/N = 2). The cross-talk between adjacent capillaries is less than 0.2%. Simultaneous analysis of 96 samples is demonstrated. PMID:21662842

  10. HI Absorption Lines Detected from the Arecibo Legacy Fast ALFA Survey Data

    Science.gov (United States)

    Zhong-zu, Wu; Martha P, Haynes; Riccardo, Giovanelli; Ming, Zhu; Ru-rong, Chen

    2015-10-01

    We present some preliminary results of an on-going study of HI 21-cm absorption lines based on the 40% survey data released by the Arecibo Legacy Fast Arecibo L-band Feed Array (ALFALFA). (1) Ten HI candidate absorbers have been detected. Five of them are previously published in the literature, and the rest of them are new detections that need further confirmation. (2) For those sources with no detected absorptions, we have calculated the upper limit of their foreground HI column density NHI. The statistical result of the NHI distribution indicates that the ratio Ts/f between the averaged spin temperature and coverage factor for DLAs (the damped Lyα systems) might be larger than 500 K. The radio frequency interference (RFI) and standing wave are the main factors affecting the detection of HI absorption lines, which have been analyzed and discussed as well in order to find a method of solution. Our study can serve as a pathfinder for the future large-scale search of HI 21-cm absorption lines using the Five-Hundred-Meter Aperture Spherical Radio Telescope (FAST), which is an Arecibo-type radio telescope currently under construction in China with greatly increased sensitivity, bandwidth, and observational sky area. As prospects, we have discussed two types of observational studies of HI absorption lines toward extragalactic sources using the FAST telescope.

  11. In-house validation of a method for determination of silver nanoparticles in chicken meat based on asymmetric flow field-flow fractionation and inductively coupled plasma mass spectrometric detection

    DEFF Research Database (Denmark)

    Löschner, Katrin; Navratilova, Jana; Grombe, Ringo;

    2015-01-01

    spectrometric detection (AF4-ICP-MS) was applied for quantitative analysis of silver nanoparticles (AgNPs) in a chicken meat matrix following enzymatic sample preparation. For the first time an analytical validation of nanoparticle detection in a food matrix by AF4-ICP-MS has been carried out and the results......Nanomaterials are increasingly used in food production and packaging, and validated methods for detection of nanoparticles (NPs) in foodstuffs need to be developed both for regulatory purposes and product development. Asymmetric flow field-flow fractionation with inductively coupled plasma mass...... showed repeatable and intermediately reproducible determination of AgNP mass fraction and size. The findings demonstrated the potential of AF4-ICP-MS for quantitative analysis of NPs in complex food matrices for use in food monitoring and control. The accurate determination of AgNP size distribution...

  12. Novel algorithm for simultaneously detecting multiple vapor materials with multiple-wavelength differential absorption lidar

    Institute of Scientific and Technical Information of China (English)

    Shirong Yin; Weiran Wang

    2006-01-01

    Differential absorption lidar (DIAL) has been successfully used to detect vapor material, however limited to detect single vapor using two closely spaced wavelengths. The progress in multiple-wavelength lasers motivates the need for detection and estimation algorithms that have the capability for simultaneous detection of multiple materials. In this paper, a simple and accurate algorithm is presented for simultaneously detecting and estimating multiple vapor materials with multiple-wavelength DIAL, which based on the maximum likelihood estimation (MLE) methodology. The performance of the algorithm is evaluated by simulation experiments, the results show that this algorithm can separately identify and quantify vapor material in mixtures and perform quite well.

  13. Infrared differential absorption lidar for stand-off detection of chemical agents

    Indian Academy of Sciences (India)

    A K Razdan; S Veerabuthiran; M K Jindal; R K Sharma

    2014-02-01

    A compact trolley-mounted pulsed transverse electric atmospheric pressure (TEA) carbon dioxide laser-based differential absorption lidar (DIAL) system capable of stand-off detection of chemical clouds in aerosol and vapour form upto about 200 m range in the atmosphere has been developed and assembled at Laser Science and Technology Centre (LASTEC), Delhi. The system was tested successfully with diethyl ether (DEE) (a toxic industrial chemical (TIC)) and differential absorption signals at on (strong absorption, 9R16) and off (weak absorption, 10R26) wavelengths were recorded for stand-off distances upto ∼100 m (open air ground path). This paper discusses the technical details of trolley-mounted CO2 DIAL system and the data generated during the test and evaluation of this sensor using DEE aerosols.

  14. Spectrometric characteristics of polystyrene scintillation films

    CERN Document Server

    Astvatsaturov, A R; Gavalyan, V B; Gavalyan, V G

    1999-01-01

    The spectrometric characteristics of five types of polystyrene scintillation films with thicknesses of 10, 30, 50 and 80 mu m and of analogous 250 mu m thick plates irradiated with sup 2 sup 3 sup 9 Pu, sup 2 sup 3 sup 8 Pu and sup 2 sup 2 sup 6 Ra sources of alpha-particles have been studied. The prospects of utilization of scintillation films as radiators for detection of heavy charged particles and measurement of their energy was experimentally shown.

  15. Absorption of human skin and its detecting platform in the process of laser cosmetology

    Science.gov (United States)

    Zhang, Yong-Lin; Ouyang, Li; Wang, Yang

    2000-10-01

    Because of the melanin, hemoglobin and water molecules, etc. contained, light absorption of human skin tissue changes with wavelength of light. This is the principle used in laser cosmetology for treating pigment diseases and vascular lesion diseases as well as skin decoration such as body tattooing, eyebrow tattooing, etc. The parameters of treatment used in laser cosmetology principally come from the research of the skin tissue optical characteristics of whites, and it is not suitable for the Oriental. The absorption spectrum of yellow race alive skin has been researched. The detecting platform for use in the measuring of vivi-tissue absorption spectrum has been developed which using opto-electronic nondestructive testing and virtual instrument techniques. The degree of pathological changes of skin can be detected by this platform also, thus the shortcoming of dosage selection in laser clinical treatments which have been decided only by naked eye observation and past experience of doctors can be solved.

  16. Spectrometric techniques 2

    CERN Document Server

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume II provides information pertinent to vacuum ultraviolet techniques to complete the demonstration of the diversity of methods available to the spectroscopist interested in the ultraviolet visible and infrared spectral regions. This book discusses the specific aspects of the technique of Fourier transform spectroscopy.Organized into five chapters, this volume begins with an overview of the large number of systematic effects in the recording of an interferogram. This text then examines the design approach for a Fourier transform spectrometer with focus on optics.

  17. Detection of Ca II absorption triplet in a circumnuclear H II region of NGC 3310

    OpenAIRE

    Terlevich, Elena; Angeles I. Díaz; Pastoriza, Miriani G.; Terlevich, Roberto; Dottori, Horacio

    1990-01-01

    This is an electronic version of an article published in Monthly Notices of the Royal Astronomical Society. Terlevich, E., Díaz, A.I., Pastoriza, M.G., Terlevich, R. and H. Dottori. Detection of Ca II absorption triplet in a circumnuclear H II region of NGC 3310. Monthly Notices of the Royal Astronomical Society 242 (1990): 48-51

  18. [The principle and technical analysis of methane detection using infrared absorption spectroscopy].

    Science.gov (United States)

    Zhang, Yu; Wang, Yi-Ding; Li, Li; Zheng, Chuan-Tao; An, Yu-Peng; Song, Zhen-Yu

    2008-11-01

    There has been considerable interest recently in methane sensor based on infrared absorption spectroscopy for industrial detection and environment monitoring. The present paper presents the intensites of methane mid-infrared fundamental absorption bands, near-infrared combination band of v2 + 2v3 and overtone band of 2v3, and it was found that the absorption strengths of fundamental bands are two orders of magnitude higher than those of overtone bands and three orders of magnitude higher than those of the combinations. Theoretically, mid-infrared detection system is much better. However, because the near-infrared source and detector are more maturely developed and cheaper, near-infrared technology is widely used. Furthermore, the near-infrared radiation can be transmitted through ordinary low-loss silica fiber, suitable for long-distance methane sensing system, meeting the needs of industrial mining and other aspects. But with the development of mid-infrared detector and high-power high-sensitivity devices, low priced micro sensor modules will be more and more developed. The development of optical methane sensors is reported in this paper. Several detection technologies were investigated such as differential absorption, harmonic detection, cavity spectroscopy enhancement and photoacoustic spectroscopy. The theoretical formula, sensitivity and system structure of these technologies are presented. PMID:19271479

  19. OH detection by absorption of frequency-doubled diode laser radiation at 308nm

    OpenAIRE

    Barry, Hugh R.; Bakowski, Ben; Corner, Laura; Freegarde, Tim; Hawkins, Oliver T. W.; Hancock, Gus; Jacobs, Robert M. J.; Peverall, Robert; Ritchie, Grant A.D.

    2000-01-01

    Radiation at 308 nm has been obtained by frequency doubling the output of a commercial diode laser cooled to 165 K. A single pass through a crystal of LiIO3 converted 1 mW of 616 nm radiation to 50 pW of UV, and this was used to detect the OH radical in absorption in a flow tube. Possible extensions of the method for detection of OH in the atmosphere are discussed.

  20. Expanding analytical possibilities concerning the detection of stanozolol misuse by means of high resolution/high accuracy mass spectrometric detection of stanozolol glucuronides in human sports drug testing.

    Science.gov (United States)

    Schänzer, Wilhelm; Guddat, Sven; Thomas, Andreas; Opfermann, Georg; Geyer, Hans; Thevis, Mario

    2013-01-01

    Anabolic-androgenic steroids (AAS) represent one of the most frequently detected classes of prohibited substances in doping controls. Due to their long-lasting beneficial effects on athletic performance, utmost retrospectivity via urine analysis is desirable and accomplished by targeting long-term metabolites of the respective drugs. In case of stanozolol, a substantial variety of metabolites has enabled the identification of numerous adverse analytical findings in the past, and recent studies concerning complementary phase-I and phase-II metabolites has further expanded the windows of opportunity for detecting the abuse of stanozolol. In this study, the utility of liquid chromatography-high resolution/high accuracy (tandem) mass spectrometry (LC-MS/MS) for the detection of 3'-OH-stanozolol glucuronide in sports drug testing is presented and the identification of two additional and so far unreported metabolites is shown. The structures of the complementary glucuronic acid conjugates were attributed to stanozolol-N-glucuronide and 17-epistanozolol-N-glucuronide. By means of chemical synthesis, stanozolol-N-glucuronide was prepared and used to corroborate the suggested structures. The 3'-OH-stanozolol glucuronide and the newly identified target compounds were implemented into routine sports drug test assays consisting of direct injection LC-MS/MS or solid-phase extraction (SPE) followed by LC-MS/MS. A considerably expanded detection window for stanozolol abuse was demonstrated compared to the use of conventional phase-I metabolites and methodologies based on, for example, low resolution LC-MS/MS or gas chromatography-tandem mass spectrometry (GC-MS/MS). The commercial availability of 3'-OH-stanozolol glucuronide has been of great value for confirmatory purposes, and 17-epistanozolol-N-glucuronide was found to be a favourable long-term metabolite for doping controls as it was observed up to 28 days post-administration of the drug. Applying the established

  1. Non-degenerate two photon absorption enhancement for laser dyes by precise lock-in detection

    International Nuclear Information System (INIS)

    This study demonstrates a measurement system for a non-degenerate two-photon absorption (NDTPA) spectrum. The NDTPA light sources are a white light super continuum beam (WLSC, 500 ∼ 720 nm) and a fundamental beam (798 nm) from a Ti:Sapphire laser. A reliable broadband NDTPA spectrum is acquired in a single-shot detection procedure using a 128-channel lock-in amplifier. The NDTPA spectra for several common laser dyes are measured. Two photon absorption cross section enhancements are found in the experiment and validated by theoretical calculation for all of the chromophores

  2. Non-degenerate two photon absorption enhancement for laser dyes by precise lock-in detection

    Energy Technology Data Exchange (ETDEWEB)

    Xue, B. [Advanced Ultrafast Laser Research Center and Department of Engineering Science, Faculty of Informatics and Engineering, University of Electro-Communications, 1-5-1 Chofugaoka, Chofu, Tokyo, 182-8585 (Japan); Japan Science and Technology Agency, CREST, 5 Sanbancho, Chiyoda-ku, Tokyo, 102-0075 (Japan); Katan, C. [Institut des Sciences Chimiques de Rennes, UMR 6226 CNRS-Université Rennes 1, 35042 Rennes (France); Bjorgaard, J. A. [Center for Nonlinear Studies, Los Alamos National Laboratory, Los Alamos, NM (United States); Theoretical Division, Los Alamos National Laboratory, Los Alamos, NM (United States); Kobayashi, T., E-mail: kobayashi@ils.uec.ac.jp [Advanced Ultrafast Laser Research Center and Department of Engineering Science, Faculty of Informatics and Engineering, University of Electro-Communications, 1-5-1 Chofugaoka, Chofu, Tokyo, 182-8585 (Japan); Japan Science and Technology Agency, CREST, 5 Sanbancho, Chiyoda-ku, Tokyo, 102-0075 (Japan); Department of Electrophysics, National Chiao-Tung University, Hsinchu, 30010, Taiwan (China); Institute of Laser Engineering, Osaka University, 2-6 Yamada-oka, Suita, Osaka, 565-0871 (Japan)

    2015-12-15

    This study demonstrates a measurement system for a non-degenerate two-photon absorption (NDTPA) spectrum. The NDTPA light sources are a white light super continuum beam (WLSC, 500 ∼ 720 nm) and a fundamental beam (798 nm) from a Ti:Sapphire laser. A reliable broadband NDTPA spectrum is acquired in a single-shot detection procedure using a 128-channel lock-in amplifier. The NDTPA spectra for several common laser dyes are measured. Two photon absorption cross section enhancements are found in the experiment and validated by theoretical calculation for all of the chromophores.

  3. [Detection technology of methane gas concentration based on infrared absorption spectrum].

    Science.gov (United States)

    Luo, Da-Feng; Yang, Jian-Hua; Zhong, Chong-Gui

    2011-02-01

    According to the disadvantages of current methane sensor in coal mine, the infrared methane concentration detection system based on the principle of infrared spectrum absorption was designed using differential absorption technology. In the system single light beam absorbing cell and single light beam and double wavelengths technology are adopted. Differential amplifier circuit serves as the core of faint signal processing circuit that detects the output signal of methane concentration, and linear formula fits the curve of methane concentration and output voltage, which realizes accurate and full range detection of gas concentration. Experiment shows that measurement error is less than 2%, and the system has very high measurement precision and possesses the basis of industrial applications. PMID:21510386

  4. Comparison of serum copper determination by colorimetric and atomic absorption spectrometric methods in seven different laboratories. The S.F.B.C. (Société Française de Biologie Clinique) Trace Element Group.

    Science.gov (United States)

    Arnaud, J; Chappuis, P; Zawislak, R; Houot, O; Jaudon, M C; Bienvenu, F; Bureau, F

    1993-02-01

    An interlaboratory collaborative trial was conducted on the determination of serum copper using two different methods, based on colorimetry (test combination Copper, Boehringer Mannheim, Mannheim, Germany) and flame atomic absorption spectrometry (FAAS). The general performance of the colorimetric method was below that of FAAS, except for sensitivity and linear range, as assessed by detection limit (0.44 versus 1.32 mumol/L) and upper limit of linearity (150 versus 50 mumol/L). The range of the between-run CVs and the recovery of standard additions were, respectively, 2.3-11.9% and 92-127% for the colorimetric method and 1.1-6.0% and 93-101% for the FAAS method. Interferences were minimal with both methods. The two techniques correlated satisfactorily (the correlation coefficients ranged from 0.945-0.970 among laboratories) but the colorimetric assay exhibited slightly higher results than the FAAS method. Each method was transferable among laboratories.

  5. Commercial Applications of X Ray Spectrometric Techniques

    International Nuclear Information System (INIS)

    In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z ≥ 10, with a few instruments capable of detecting also elements with Z ≥ 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg’s law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

  6. 运用HPLC-MS对鸦胆子油自微乳给药系统肠吸收的研究%High-performance Liquid Chromatography Coupled with Mass Spectrometric Method for the Intestinal Absorption Study of Brucea Javanica Oil SMEDDS

    Institute of Scientific and Technical Information of China (English)

    陈瑾瑾; 张懿; 王睿锐; 李盈; 沈琦; 马依然

    2012-01-01

    Objective: To develop a rapid, sensitive and selective high-performance liquid chromatography coupled with mass spectrometric method (HPLC-MS) for detection oleic acid and linoleic acid. Methods: The chromatographic separation was achieved on C18 column at 35℃, with a mobile phase consisting of methanol-distilled water (95:5, v/v) at a flow rate of 0.4 mL/min. An in-vitro diffusion chamber system across isolated rat intestinal membranes was chosen as a model. A self-microemulsifying drug delivery system was used to enhance the intestinal absorption of bruces javanica oil. Results: Oleic acid and linoleic acid were separated with retention times of 10.46 ± 0.02 and 8.55 ± 0.01 min, respectively. A good linear relationship for oleic acid and linoleic acid were in the range of 0.50~50.0 ng/mL(oleic acid) and 5.06~101.2 ng/mL(linoleic acid) , respectively. The mean absolute recoveries of oleic acid and linoleic acid determined in middle concentrations were 97.49± 3.11 % and 105.76± 3.13 % respectively. The coefficients of variation for inter-day and intra-day assay were less than 5 %. The absorption of oleic acid and linoleic acid in bruces javanica oil were 2.8-fold and 4.1-fold enhancement in the presence of the self-microemulsifying drug delivery system respectively, compared with brucea javanica oil alone. Conclusion: HPLC-MS method will be of great utility in routine quality control procedure for the determination of oleic acid and linoleic acid in absorption experiments.%目的:建立高效液相色谱-串联质谱法检测油酸和亚油酸含量的方法,从而对鸦胆子油自微乳给药系统中鸦胆子油的肠吸收进行研究.方法:以甲醇-水(95∶5 v/v)为流动相,流速为0.4 mL/min,柱温为35℃作为高效液相色谱的检测条件.利用大鼠小肠膜建立体外药物扩散体系研究鸦胆子油的肠吸收特性.结果:油酸和亚油酸的保留时间分别为10.46± 0.02和8.55±0.01 min,线性范围分别为0.50~50.0 ng

  7. Determination of 2-ethylhexyl 4-(dimethylamino) benzoate using membrane-assisted liquid-liquid extraction and gas chromatography-mass spectrometric detection.

    Science.gov (United States)

    March, J G; Genestar, C; Simonet, B M

    2009-06-01

    A flow-cell for micro-porous membrane liquid-liquid extraction with a sheet membrane was used to extract 2-ethylhexyl 4-(dimethylamino) benzoate (EDB) from urine of solar-cream users and spiked wine samples. The cell enabled the target analyte to be extracted from 7.9 mL of donor solution into 200 microL of acceptor solution (decane). After extraction, the acceptor solution was transferred to a micro-vial for GC-MS analysis without derivation. In this work, variables affecting the enrichment factor were also studied, such as organic solvent, extraction time, recirculation flow of the donor solution through the donor chamber, presence of potassium chloride and ethanol in the donor solution and pH. The method has been evaluated in terms of linearity, sensitivity, precision, limits of detection and quantification and extraction efficiency. Limits of quantification were 1 and 3 microg L(-1) EDB for urine and wine, respectively. Quantitative analysis has been carried out by applying the method of standard additions. Within- and between-day relative standard deviations were lower than 12% and 20%, respectively. EDB was found in the urine of users of cream containing EDB in the concentration interval 1.2-7.2 microg L(-1). Therefore, this provides evidence of EDB dermal absorption and subsequent excretion through the urinary tract. EDB was not found in the analysed wine samples. PMID:19347661

  8. Development and validation of a supercritical fluid chromatography method for the direct determination of enantiomeric purity of provitamin B5 in cosmetic formulations with mass spectrometric detection.

    Science.gov (United States)

    Khater, Syame; West, Caroline

    2015-01-01

    A rapid and efficient chiral supercritical fluid chromatography (SFC) method has been developed for the quantitative determination of panthenol enantiomers in cosmetic formulations (cream, lotion, wipe, and exfoliant). Indeed, the pharmacological effect only depends on the D form (Dexpanthenol) thus accurate measurement of its enantiomeric purity in formulated cosmetic products is of interest. The samples were prepared with liquid-liquid extraction followed by solid-phase extraction on Adsorbex amino cartridges. After testing several enantioselective columns in an attempt at reversing the elution order to have the minor enantiomer eluted first, the best separation of enantiomers and internal standard (N-acetyl-L-alanine) was achieved on a 3 μm-amylose-type immobilized polysaccharide chiral stationary phase (Chiralpak IA) in less than 6 min with a simple mobile phase comprising carbon dioxide and 11% methanol pumped at 2.3 mL/min, 25°C and 150 bar backpressure. Supercritical fluid chromatography coupled to both an optical diode-array detector and a user-friendly single-quadrupole mass spectrometer (Waters QDa) equipped with electrospray ionization source has been used. The on-line coupling ensures the technique to be more informative and improves detection sensitivity, as underivatized panthenol has a poor UV absorption. The limit of quantification (LOQ) achieved with single-ion recording was 0.5 μg/mL. The method was validated in terms of linearity, precision and accuracy and satisfactory results were obtained. PMID:25459930

  9. [Study on experiment of absorption spectroscopy detection of pesticide residues of carbendazim in orange juice].

    Science.gov (United States)

    Ji, Ren-Dong; Chen, Meng-Lan; Zhao, Zhi-Min; Zhu, Xing-Yue; Wang, Le-Xin; Liu, Quan-Jin

    2014-03-01

    Absorption spectra were studied for the carbendazim, in the mixed solution of orange juice and carbendazim using spectrophotometer. The most intensive characteristic peak (285 nm) was found in the spectrum of carbendazim standard solution. Compared with the carbendazim drug solution, the peak position of absorption spectrum has the blue shift (285-280 nm) when carbendazim (0.28 mg x mL(-1))was added in the orange juice. So that we can conclude that interaction happened between the orange juice and carbendazim. Through the method of least squares fitting, the prediction models between the absorbance of orange juice and carbendazim content was obtained with a good linear relationship. The linear function model was: I = 2.41 + 9.26x, the correlation coefficient was 0.996, and the recovery was: 81%-102%. According to the regression model, we can obtain the amount of carbendazim pesticide residues in orange juice. It was verified that the method of using ultraviolet-visible absorption spectra was feasible to detect the carbendazim residues in orange juice. The result proved that it is possible to detect pesticide residues of carbendazim in orange juice, and it can meet the needs of rapid analysis. This study provides a new way for the detection of pesticide residues.

  10. Detection of water vapour absorption around 363nm in measured atmospheric absorption spectra and its effect on DOAS evaluations

    Science.gov (United States)

    Lampel, Johannes; Polyansky, Oleg. L.; Kyuberis, Alexandra A.; Zobov, Nikolai F.; Tennyson, Jonathan; Lodi, Lorenzo; Pöhler, Denis; Frieß, Udo; Platt, Ulrich; Beirle, Steffen; Wagner, Thomas

    2016-04-01

    Water vapour is known to absorb light from the microwave region to the blue part of the visible spectrum at a decreasing magnitude. Ab-initio approaches to model individual absorption lines of the gaseous water molecule predict absorption lines until its dissociation limit at 243 nm. We present first evidence of water vapour absorption at 363 nm from field measurements based on the POKAZATEL absorption line list by Polyansky et al. (2016) using data from Multi-Axis differential optical absorption spectroscopy (MAX-DOAS) and Longpath (LP)-DOAS measurements. The predicted absorptions contribute significantly to the observed optical depths with up to 2 × 10‑3. Their magnitude correlates well (R2 = 0.89) to simultaneously measured well-established water vapour absorptions in the blue spectral range from 452-499 nm, but is underestimated by a factor of 2.6 ± 0.6 in the ab-initio model. At a spectral resolution of 0.5nm this leads to a maximum absorption cross-section value of 5.4 × 10‑27 cm2/molec at 362.3nm. The results are independent of the employed cross-section data to compensate for the overlayed absorption of the oxygen dimer O4. The newly found absorption can have a significant impact on the spectral retrieval of absorbing trace-gas species in the spectral range around 363 nm. Its effect on the spectral analysis of O4, HONO and OClO are discussed.

  11. Detection of Ca II absorption triplet in a circumnuclear H II region of NGC 3310

    International Nuclear Information System (INIS)

    We have obtained long slit spectrophotometry across NGC 3310, a luminous galaxy with circumnuclear bursts of star formation, covering the spectral range from λ3650 to 9700 A. In one giant star-forming region, the near-IR Ca II absorption lines (a signature of young supergiants) was detected with a strength similar to that of the nuclear region. This is, to our knowledge, the first detection of the IR Ca II triplet in an extragalactic giant H II region and confirms theoretical predictions that, after some 4 Myr, red supergiants should appear in bursts of star formation. (author)

  12. Wavelength modulation spectroscopy--digital detection of gas absorption harmonics based on Fourier analysis.

    Science.gov (United States)

    Mei, Liang; Svanberg, Sune

    2015-03-20

    This work presents a detailed study of the theoretical aspects of the Fourier analysis method, which has been utilized for gas absorption harmonic detection in wavelength modulation spectroscopy (WMS). The lock-in detection of the harmonic signal is accomplished by studying the phase term of the inverse Fourier transform of the Fourier spectrum that corresponds to the harmonic signal. The mathematics and the corresponding simulation results are given for each procedure when applying the Fourier analysis method. The present work provides a detailed view of the WMS technique when applying the Fourier analysis method.

  13. Logarithmic conversion of absorption detection in wavelength modulation spectroscopy with a current-modulated diode laser.

    Science.gov (United States)

    Wang, Yuntao; Cai, Haiwen; Geng, Jianxin; Fang, Zujie

    2009-07-20

    Logarithmic-conversion data processing used in wavelength modulation spectroscopy (WMS) with a current-modulated diode laser as its source is analyzed and compared with second-to-first ratio detection. Analytic Fourier coefficients of logarithmic-converted residual amplitude modulation (RAM) of a light source are given. An experimental setup for methane absorption detection at 1650 nm is described. It is shown theoretically and experimentally that logarithmic-converted WMS cannot only eliminate the fluctuation of received light power, but also improve the signal-to-noise ratio significantly. PMID:19623220

  14. A broadband absorption spectrometer using light emitting diodes for ultrasensitive, in situ trace gas detection

    International Nuclear Information System (INIS)

    A broadband absorption spectrometer has been developed for highly sensitive and target-selective in situ trace gas measurements. The instrument employs two distinct modes of operation: (i) broadband cavity enhanced absorption spectroscopy (BBCEAS) is used to quantify the concentration of gases in sample mixtures from their characteristic absorption features, and (ii) periodic measurements of the cavity mirrors' reflectivity are made using step-scan phase shift cavity ringdown spectroscopy (PSCRDS). The latter PSCRDS method provides a stand-alone alternative to the more usual method of determining mirror reflectivities by measuring BBCEAS absorption spectra for calibration samples of known composition. Moreover, the instrument's two modes of operation use light from the same light emitting diode transmitted through the cavity in the same optical alignment, hence minimizing the potential for systematic errors between mirror reflectivity determinations and concentration measurements. The ability of the instrument to quantify absorber concentrations is tested in instrument intercomparison exercises for NO2 (versus a laser broadband cavity ringdown spectrometer) and for H2O (versus a commercial hygrometer). A method is also proposed for calculating effective absorption cross sections for fitting the differential structure in BBCEAS spectra due to strong, narrow absorption lines that are under-resolved and hence exhibit non-Beer-Lambert law behavior at the resolution of the BBCEAS measurements. This approach is tested on BBCEAS spectra of water vapor's 4v+δ absorption bands around 650 nm. The most immediate analytical application of the present instrument is in quantifying the concentration of reactive trace gases in the ambient atmosphere. The instrument's detection limits for NO3 as a function of integration time are considered in detail using an Allan variance analysis. Experiments under laboratory conditions produce a 1σ detection limit of 0.25 pptv for a 10 s

  15. [Carbon monoxide gas detection system based on mid-infrared spectral absorption technique].

    Science.gov (United States)

    Li, Guo-Lin; Dong, Ming; Song, Nan; Song, Fang; Zheng, Chuan-Tao; Wang, Yi-Ding

    2014-10-01

    Based on infrared spectral absorption technique, a carbon monoxide (CO) detection system was developed using the fundamental absorption band at the wavelength of 4.6 μm of CO molecule and adopting pulse-modulated wideband incandescence and dual-channel detector. The detection system consists of pulse-modulated wideband incandescence, open ellipsoid light-collec- tor gas-cell, dual-channel detector, main-control and signal-processing module. By optimizing open ellipsoid light-collector gas- cell, the optical path of the gas absorption reaches 40 cm, and the amplitude of the electrical signal from the detector is 2 to 3 times larger than the original signal. Therefore, by using the ellipsoidal condenser, the signal-to-noise ratio of the system will be to some extent increased to improve performance of the system. With the prepared standard CO gas sample, sensing characteris- tics on CO gas were investigated. Experimental results reveal that, the limit of detection (LOD) is about 10 ppm; the relative er- ror at the LOD point is less than 14%, and that is less than 7. 8% within the low concentration range of 20~180 ppm; the maxi- mum absolute error of 50 min long-term measurement concentration on the 0 ppm gas sample is about 3 ppm, and the standard deviation is as small as 0. 18 ppm. Compared with the CO detection systems utilizing quantum cascaded lasers (QCLs) and dis- tributed feedback lasers (DFBLs), the proposed sensor shows potential applications in CO detection under the circumstances of coal-mine and environmental protection, by virtue of high performance-cost ratio, simple optical-path structure, etc. PMID:25739235

  16. Flame atomic absorption spectrometric determination of trace amounts of Pb(II) and Cr(III) in biological, food and environmental samples after preconcentration by modified nano-alumina

    International Nuclear Information System (INIS)

    A new solid-phase extraction sorbent was used for the preconcentration of Pb(II) and Cr(III) ions prior to their determination by flame atomic absorption spectrometry. It was prepared by immobilization of 2,4-dinitrophenylhydrazine on nano-alumina coated with sodium dodecyl sulfate. The sorbent was characterized by scanning electron microscopy, N2 adsorption and Fourier transform infrared spectrometry, and used for preconcentration and separation of Pb(II) and Cr(III) from aqueous solutions. The ions on the sorbent were eluted with a mixture of nitric acid and methanol. The effects of sample pH, flow rates of samples and eluent, type of eluent, breakthrough volume and potentially interfering ions were studied. Linearity is maintained between 1.2 and 350 μg L-1 of Pb(II), and between 2.4 and 520 μg L-1 of Cr(III) for an 800-mL sample. The detection limit (3 s, N=10) for Pb(II) and Cr(III) ions is 0.43 and 0.55 μg L-1, respectively, and the maximum preconcentration factor is 267. The method was successfully applied to the evaluation of these trace and toxic metals in various water, food, industrial effluent and urine samples. (author)

  17. Invisible Active Galactic Nuclei. II Radio Morphologies & Five New HI 21 cm Absorption Line Detections

    CERN Document Server

    Yan, Ting; Darling, Jeremy; Momjian, Emmanuel; Sharma, Soniya; Kanekar, Nissim

    2015-01-01

    We have selected a sample of 80 candidates for obscured radio-loud active galactic nuclei and presented their basic optical/near-infrared (NIR) properties in Paper 1. In this paper, we present both high-resolution radio continuum images for all of these sources and HI 21cm absorption spectroscopy for a few selected sources in this sample. A-configuration 4.9 and 8.5 GHz VLA continuum observations find that 52 sources are compact or have substantial compact components with size 0.1 Jy at 4.9 GHz. The most compact 36 sources were then observed with the VLBA at 1.4 GHz. One definite and 10 candidate Compact Symmetric Objects (CSOs) are newly identified, a detection rate of CSOs ~3 times higher than the detection rate previously found in purely flux-limited samples. Based on possessing compact components with high flux densities, 60 of these sources are good candidates for absorption-line searches. Twenty seven sources were observed for HI 21cm absorption at their photometric or spectroscopic redshifts with only ...

  18. HI emission and absorption in nearby, gas-rich galaxies II. -- sample completion and detection of intervening absorption in NGC 5156

    CERN Document Server

    Reeves, S N; Allison, J R; Koribalski, B S; Curran, S J; Pracy, M B; Phillips, C J; Bignall, H E; Reynolds, C

    2016-01-01

    We present the results of a survey for intervening 21cm HI absorption in a sample of 10 nearby, gas-rich galaxies selected from the HI Parkes All-Sky Survey (HIPASS). This follows the six HIPASS galaxies searched in previous work and completes our full sample. In this paper we searched for absorption along 17 sightlines with impact parameters between 6 and 46 kpc, making one new detection. We also obtained simultaneous HI emission-line data, allowing us to directly relate the absorption-line detection rate to the HI distribution. From this we find the majority of the non-detections in the current sample are because sightline does not intersect the HI disc of the galaxy at sufficiently high column density, but that source structure is also an important factor. The detected absorption-line arises in the galaxy NGC 5156 ($z = 0.01$) at an impact parameter of 19 kpc. The line is deep and narrow with an integrated optical depth of 0.82 km s$^{-1}$. High resolution Australia Telescope Compact Array (ATCA) images at...

  19. WSRT detection of HI absorption in the z=3.4 damped Ly alpha system in PKS 0201+113

    NARCIS (Netherlands)

    deBruyn, AG; ODea, CP; Baum, SA

    1996-01-01

    We report the detection of a faint narrow HI absorption line at a redshift of 3.38 against the quasar PKS 0201+113 which itself has an emission redshift of 3.61. The absorption line redshift agrees, to within the errors, with that of a damped Ly alpha line. The line has a halfwidth of about 9 km s(-

  20. Quantum cascade laser-based multipass absorption system for hydrogen peroxide detection

    Science.gov (United States)

    Cao, Yingchun; Sanchez, Nancy P.; Jiang, Wenzhe; Ren, Wei; Lewicki, Rafal; Jiang, Dongfang; Griffin, Robert J.; Tittel, Frank K.

    2015-01-01

    Hydrogen peroxide (H2O2) is a relevant molecular trace gas species, that is related to the oxidative capacity of the atmosphere, the production of radical species such as OH, the generation of sulfate aerosol via oxidation of S(IV) to S(VI), and the formation of acid rain. The detection of atmospheric H2O2 involves specific challenges due to its high reactivity and low concentration (ppbv to sub-ppbv level). Traditional methods for measuring atmospheric H2O2 concentration are often based on wet-chemistry methods that require a transfer from the gas- to liquid-phase for a subsequent determination by techniques such as fluorescence spectroscopy, which can lead to problems such as sampling artifacts and interference by other atmospheric constituents. A quartz-enhanced photoacoustic spectroscopy-based system for the measurement of atmospheric H2O2 with a detection limit of 75 ppb for 1-s integration time was previously reported. In this paper, an updated H2O2 detection system based on long-optical-path-length absorption spectroscopy by using a distributed feedback quantum cascade laser (DFB-QCL) will be described. A 7.73-μm CW-DFB-QCL and a thermoelectrically cooled infrared detector, optimized for a wavelength of 8 μm, are employed for theH2O2 sensor system. A commercial astigmatic Herriott multi-pass cell with an effective optical path-length of 76 m is utilized for the reported QCL multipass absorption system. Wavelength modulation spectroscopy (WMS) with second harmonic detection is used for enhancing the signal-to-noise-ratio. A minimum detection limit of 13.4 ppb is achieved with a 2 s sampling time. Based on an Allan-Werle deviation analysis the minimum detection limit can be improved to 1.5 ppb when using an averaging time of 300 s.

  1. Herschel-HIFI detections of hydrides towards AFGL 2591 (Envelope emission versus tenuous cloud absorption)

    CERN Document Server

    Bruderer, S; van Dishoeck, E F; Melchior, M; Doty, S D; van der Tak, F; Stäuber, P; Wampfler, S F; Dedes, C; Yıldız, U A; Pagani, L; Giannini, T; de Graauw, Th; Whyborn, N; Teyssier, D; Jellema, W; Shipman, R; Schieder, R; Honingh, N; Caux, E; Bächtold, W; Csillaghy, A; Monstein, C; Bachiller, R; Baudry, A; Benedettini, M; Bergin, E; Bjerkeli, P; Blake, G A; Bontemps, S; Braine, J; Caselli, P; Cernicharo, J; Codella, C; Daniel, F; di Giorgio, A M; Dominik, C; Encrenaz, P; Fich, M; Fuente, A; Goicoechea, J R; Helmich, F; Herczeg, G J; Herpin, F; Hogerheijde, M R; Jacq, T; Johnstone, D; Jørgensen, J K; Kristensen, L E; Larsson, B; Lis, D; Liseau, R; Marseille, M; McCoey, C; Melnick, G; Neufeld, D; Nisini, B; Olberg, M; Parise, B; Pearson, J C; Plume, R; Risacher, C; Santiago-Garcia, J; Saraceno, P; Shipman, R; Tafalla, M; van Kempen, T A; Visser, R; Wyrowski, F

    2010-01-01

    The Heterodyne Instrument for the Far Infrared (HIFI) onboard the Herschel Space Observatory allows the first observations of light diatomic molecules at high spectral resolution and in multiple transitions. Here, we report deep integrations using HIFI in different lines of hydrides towards the high-mass star forming region AFGL 2591. Detected are CH, CH+, NH, OH+, H2O+, while NH+ and SH+ have not been detected. All molecules except for CH and CH+ are seen in absorption with low excitation temperatures and at velocities different from the systemic velocity of the protostellar envelope. Surprisingly, the CH(JF,P = 3/2_2,- - 1/2_1,+) and CH+(J = 1 - 0, J = 2 - 1) lines are detected in emission at the systemic velocity. We can assign the absorption features to a foreground cloud and an outflow lobe, while the CH and CH+ emission stems from the envelope. The observed abundance and excitation of CH and CH+ can be explained in the scenario of FUV irradiated outflow walls, where a cavity etched out by the outflow al...

  2. Mid-infrared carbon monoxide detection system using differential absorption spectroscopy technique

    Science.gov (United States)

    Dong, Ming; Sui, Yue; Li, Guo-lin; Zheng, Chuan-tao; Chen, Mei-mei; Wang, Yi-ding

    2015-11-01

    A differential carbon monoxide (CO) concentration sensing device using a self-fabricated spherical mirror (e.g. light-collector) and a multi-pass gas-chamber is presented in this paper. Single-source dual-channel detection method is adopted to suppress the interferences from light source, optical path and environmental changes. Detection principle of the device is described, and both the optical part and the electrical part are developed. Experiments are carried out to evaluate the sensing performance on CO concentration. The results indicate that at 1.013×105 Pa and 298 K, the limit of detection (LoD) is about 11.5 mg/m3 with an absorption length of 40 cm. As the gas concentration gets larger than 115 mg/m3 (1.013×105 Pa, 298 K), the relative detection error falls into the range of -1.7%—+1.9%. Based on 12 h long-term measurement on the 115 mg/m3 and 1 150 mg/m3 CO samples, the maximum detection errors are about 0.9% and 5.5%, respectively. Due to the low cost and competitive characteristics, the proposed device shows potential applications in CO detection in the circumstances of coal-mine production and environmental protection.

  3. Herschel observations of extra-ordinary sources: Detecting spiral arm clouds by CH absorption lines

    CERN Document Server

    Qin, S -L; Comito, C; Möller, T; Rolffs, R; Müller, H S P; Belloche, A; Menten, K M; Lis, D C; Phillips, T G; Bergin, E A; Bell, T A; Crockett, N R; Blake, G A; Cabrit, S; Caux, E; Ceccarelli, C; Cernicharo, J; Daniel, F; Dubernet, M -L; Emprechtinger, M; Encrenaz, P; Falgarone, E; Gerin, M; Giesen, T F; Goicoechea, J R; Goldsmith, P F; Gupta, H; Herbst, E; Joblin, C; Johnstone, D; Langer, W D; Lord, S D; Maret, S; Martin, P G; Melnick, G J; Morris, P; Murphy, J A; Neufeld, D A; Ossenkopf, V; Pagani, L; Pearson, J C; Pérault, M; Plume, R; Salez, M; Schlemmer, S; Stutzki, J; Trappe, N; van der Tak, F F S; Vastel, C; Wang, S; Yorke, H W; Yu, S; Zmuidzinas, J; Boogert, A; Güsten, R; Hartogh, P; Honingh, N; Karpov, A; Kooi, J; Krieg, J M; Schieder, R; Diez-Gonzalez, M C; Bachille, R; Martin-Pintado, J; Baechtold, W; Olberg, M; Nordh, L H; Gill, J L; Chattopadhyay, G

    2010-01-01

    We have observed CH absorption lines ($J=3/2, N=1 \\leftarrow J=1/2, N=1$) against the continuum source Sgr~B2(M) using the \\textit{Herschel}/HIFI instrument. With the high spectral resolution and wide velocity coverage provided by HIFI, 31 CH absorption features with different radial velocities and line widths are detected and identified. The narrower line width and lower column density clouds show `spiral arm' cloud characteristics, while the absorption component with the broadest line width and highest column density corresponds to the gas from the Sgr~B2 envelope. The observations show that each `spiral arm' harbors multiple velocity components, indicating that the clouds are not uniform and that they have internal structure. This line-of-sight through almost the entire Galaxy offers unique possibilities to study the basic chemistry of simple molecules in diffuse clouds, as a variety of different cloud classes are sampled simultaneously. We find that the linear relationship between CH and H$_2$ column dens...

  4. [Study of the Detecting System of CH4 and SO2 Based on Spectral Absorption Method and UV Fluorescence Method].

    Science.gov (United States)

    Wang, Shu-tao; Wang, Zhi-fang; Liu, Ming-hua; Wei, Meng; Chen, Dong-ying; Wang, Xing-long

    2016-01-01

    According to the spectral absorption characteristics of polluting gases and fluorescence characteristics, a time-division multiplexing detection system is designed. Through this system we can detect Methane (CH4) and sulfur dioxide (SO2) by using spectral absorption method and the SO2 can be detected by using UV fluorescence method. The system consists of four parts: a combination of a light source which could be switched, the common optical path, the air chamber and the signal processing section. The spectral absorption characteristics and fluorescence characteristics are measured first. Then the experiment of detecting CH4 and SO2 through spectral absorption method and the experiment of detecting SO2 through UV fluorescence method are conducted, respectively. Through measuring characteristics of spectral absorption and fluorescence, we get excitation wavelengths of SO2 and CH4 measured by spectral absorption method at the absorption peak are 280 nm and 1.64 μm, respectively, and the optimal excitation wavelength of SO2 measured by UV fluorescence method is 220 nm. we acquire the linear relation between the concentration of CH4 and relative intensity and the linear relation between the concentration of SO2 and output voltage after conducting the experiment of spectral absorption method, and the linearity are 98.7%, 99.2% respectively. Through the experiment of UV fluorescence method we acquire that the relation between the concentration of SO2 and the voltage is linear, and the linearity is 99.5%. Research shows that the system is able to be applied to detect the polluted gas by absorption spectrum method and UV fluorescence method. Combing these two measurement methods decreases the costing and the volume, and this system can also be used to measure the other gases. Such system has a certain value of application. PMID:27228784

  5. [Study of the Detecting System of CH4 and SO2 Based on Spectral Absorption Method and UV Fluorescence Method].

    Science.gov (United States)

    Wang, Shu-tao; Wang, Zhi-fang; Liu, Ming-hua; Wei, Meng; Chen, Dong-ying; Wang, Xing-long

    2016-01-01

    According to the spectral absorption characteristics of polluting gases and fluorescence characteristics, a time-division multiplexing detection system is designed. Through this system we can detect Methane (CH4) and sulfur dioxide (SO2) by using spectral absorption method and the SO2 can be detected by using UV fluorescence method. The system consists of four parts: a combination of a light source which could be switched, the common optical path, the air chamber and the signal processing section. The spectral absorption characteristics and fluorescence characteristics are measured first. Then the experiment of detecting CH4 and SO2 through spectral absorption method and the experiment of detecting SO2 through UV fluorescence method are conducted, respectively. Through measuring characteristics of spectral absorption and fluorescence, we get excitation wavelengths of SO2 and CH4 measured by spectral absorption method at the absorption peak are 280 nm and 1.64 μm, respectively, and the optimal excitation wavelength of SO2 measured by UV fluorescence method is 220 nm. we acquire the linear relation between the concentration of CH4 and relative intensity and the linear relation between the concentration of SO2 and output voltage after conducting the experiment of spectral absorption method, and the linearity are 98.7%, 99.2% respectively. Through the experiment of UV fluorescence method we acquire that the relation between the concentration of SO2 and the voltage is linear, and the linearity is 99.5%. Research shows that the system is able to be applied to detect the polluted gas by absorption spectrum method and UV fluorescence method. Combing these two measurement methods decreases the costing and the volume, and this system can also be used to measure the other gases. Such system has a certain value of application.

  6. Detection of EC absorption radius for real-time control applications

    International Nuclear Information System (INIS)

    Localized ECRH/ECCD is a promising tool for a variety of applications, from Tearing Mode stabilization to sawtooth-crash triggering (or suppression), Internal Transport Barrier control and detection, heat transport studies, formation of advanced scenarios. In all cases the knowledge of the real absorption radius is important for the understanding of experimental results. In some cases, as for NTM stabilization or sawtooth control, the intervention of ECRH/ECCD should eventually be automatic and in real time in fusion reactors, requiring continuous information on the absorption radius for a correct feedback action. In case several EC beams are to be used currently, possibly each one heating a different layer, real-time detection of all absorption radii is indeed a difficult task. Well-known techniques for power deposition profile PEC(r) reconstruction are based on a fast change of the EC power and a fast measurement of the electron temperature profile. ECE diagnostic is preferable, because of the close relation between emission and absorption, and frequency instead of radius can be used as the ordering parameter. Two complementary techniques are feasible: On or Off switching ECRH with monitoring of the Te ramp-rate radial profile; modulated ECRH with monitoring of the fluctuating amplitude distribution. In both cases, in order to provide an accurate PEC(r) profile the time scale for Te measurement has to be fast, in principle much shorter than the heat diffusion time across the absorption layer δdep. Since in most cases the typical order of magnitude of the absorption layer width is δdep ∼ 0.03 m, and the thermal diffusivity is in the order of χ ∼ 1 m2/s, it follows that the characteristic diffusion time τdiff = d2/χe is in the order of a ms, and modulation frequencies in the kHz range are needed. MECH technique can in principle provide continuous monitoring of rdep, but at the expense of a non-negligible fraction of the total power available for the

  7. H I emission and absorption in nearby, gas-rich galaxies - II. Sample completion and detection of intervening absorption in NGC 5156

    Science.gov (United States)

    Reeves, S. N.; Sadler, E. M.; Allison, J. R.; Koribalski, B. S.; Curran, S. J.; Pracy, M. B.; Phillips, C. J.; Bignall, H. E.; Reynolds, C.

    2016-04-01

    We present the results of a survey for intervening 21 cm H I absorption in a sample of 10 nearby, gas-rich galaxies selected from the H I Parkes All-Sky Survey (HIPASS). This follows the six HIPASS galaxies searched in previous work and completes our full sample. In this paper, we searched for absorption along 17 sightlines with impact parameters between 6 and 46 kpc, making one new detection. We also obtained simultaneous H I emission-line data, allowing us to directly relate the absorption-line detection rate to the H I distribution. From this, we find the majority of the non-detections in the current sample are because sightline does not intersect the H I disc of the galaxy at sufficiently high column density, but that source structure is also an important factor. The detected absorption-line arises in the galaxy NGC 5156 (z = 0.01) at an impact parameter of 19 kpc. The line is deep and narrow with an integrated optical depth of 0.82 km s-1. High-resolution Australia Telescope Compact Array (ATCA) images at 5 and 8 GHz reveal that the background source is resolved into two components with a separation of 2.6 arcsec (500 pc at the redshift of the galaxy), with the absorption likely occurring against a single component. We estimate that the ratio of the spin temperature and covering factor, TS/f, is approximately 950 K in the outer disc of NGC 5156, but further observations using very long baseline interferometry would allow us to accurately measure the covering factor and spin temperature of the gas.

  8. Spectrophotometric detection of diethylstilbestrol on the basis of the plasmon resonance absorption of silver nanoparticles

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    In this study,a spectrophotometric detection method for diethylstilbestrol(DES)was proposed by reducing silver nitrate(AgNO3)to obtain silver nanoparticles(AgNPs)in the medium of ammonia and sodium hydroxide.It was found that the resulting AgNPs have plasmon resonance absorption(PRA)characteristic at 415 nm,and the PRA is proportional to the increase of DES concentration in the range of 4.0×10-8-1.0×10-5M with the detection limit(3σ)of 1.2×10-7M.Most of the coexisting substances at high concentrations did n...

  9. Infrared absorption spectroscopy of carbon monoxide on nickel films: a low temperature thermal detection technique

    Energy Technology Data Exchange (ETDEWEB)

    Bailey, R.B.

    1978-11-01

    Sensitive vibrational spectra of carbon monoxide molecules adsorbed on evaporated nickel films have been measured by attaching a thermometer to the sample, cooling the assembly to liquid helium temperatures, and recording the temperature changes which occur when infrared radiation is absorbed. The measurements are made in an ultrahigh vacuum chamber in which the sample surface can be cleaned, heated, exposed to gas molecules and cooled to 1.6 K for the infrared measurements. The spectra of chemisorbed CO molecules are interpreted in terms of the linear and bridge adsorption sites on the nickel surface, and they show how the distribution of molecules among these sites changes when the CO coverage increases and intermolecular forces become important. The spectra of physically adsorbed molecules in both monolayer and multilayer films are also reported. Absorptions as small as five parts in 10/sup 5/ of the incident radiation can presently be detected in spectra covering broad bands of infrared frequencies with a resolution of 2 cm/sup -1/. This high sensitivity is attributable to the low noise and reduced background signal of the thermal detection scheme, to the stability of the rapid scan Fourier transform infrared spectrometer, and to the automated computerized data acquisition electronics. Better performance is expected in future experiments on single crystal samples as well as evaporated films. This will make it possible to study molecules with weaker absorptions than CO and to look for evidence of chemical reactions between different adsorbed molecules.

  10. Metamaterial-enhanced vibrational absorption spectroscopy for the detection of protein molecules

    Science.gov (United States)

    Bui, Tung S.; Dao, Thang D.; Dang, Luu H.; Vu, Lam D.; Ohi, Akihiko; Nabatame, Toshihide; Lee, YoungPak; Nagao, Tadaaki; Hoang, Chung V.

    2016-01-01

    From visible to mid-infrared frequencies, molecular sensing has been a major successful application of plasmonics because of the enormous enhancement of the surface electromagnetic nearfield associated with the induced collective motion of surface free carriers excited by the probe light. However, in the lower-energy terahertz (THz) region, sensing by detecting molecular vibrations is still challenging because of low sensitivity, complicated spectral features, and relatively little accumulated knowledge of molecules. Here, we report the use of a micron-scale thin-slab metamaterial (MM) architecture, which functions as an amplifier for enhancing the absorption signal of the THz vibration of an ultrathin adsorbed layer of large organic molecules. We examined bovine serum albumin (BSA) as a prototype large protein molecule and Rhodamine 6G (Rh6G) and 3,3′-diethylthiatricarbocyanine iodide (DTTCI) as examples of small molecules. Among them, our MM significantly magnified only the signal strength of bulky BSA. On the other hand, DTTCI and Rh6G are inactive, as they lack low-frequency vibrational modes in this frequency region. The results obtained here clearly demonstrate the promise of MM-enhanced absorption spectroscopy in the THz region for detection and structural monitoring of large biomolecules such as proteins or pathogenic enzymes. PMID:27555217

  11. [The application of atomic absorption spectrometry in automatic transmission fault detection].

    Science.gov (United States)

    Chen, Li-dan; Chen, Kai-kao

    2012-01-01

    The authors studied the innovative applications of atomic absorption spectrometry in the automatic transmission fault detection. After the authors have determined Fe, Cu and Cr contents in the five groups of Audi A6 main metal in automatic transmission fluid whose travel course is respectively 10-15 thousand kilometers, 20-26 thousand kilometers, 32-38 thousand kilometers, 43-49 thousand kilometers, and 52-58 thousand kilometers by atomic absorption spectrometry, the authors founded the database of primary metal content in the Audi A6 different mileage automatic transmission fluid (ATF). The research discovered that the main metal content in the automatic transmission fluid increased with the vehicles mileage and its normal metal content level in the automatic transmission fluid is between the two trend lines. The authors determined the main metal content of automatic transmission fluid which had faulty symptoms and compared it with its database value. Those can not only judge the wear condition of the automatic transmission which had faulty symptoms but also help the automobile detection and maintenance personnel to diagnose automatic transmission failure reasons without disintegration. This reduced automobile maintenance costs, and improved the quality of automobile maintenance.

  12. Metamaterial-enhanced vibrational absorption spectroscopy for the detection of protein molecules

    Science.gov (United States)

    Bui, Tung S.; Dao, Thang D.; Dang, Luu H.; Vu, Lam D.; Ohi, Akihiko; Nabatame, Toshihide; Lee, Youngpak; Nagao, Tadaaki; Hoang, Chung V.

    2016-08-01

    From visible to mid-infrared frequencies, molecular sensing has been a major successful application of plasmonics because of the enormous enhancement of the surface electromagnetic nearfield associated with the induced collective motion of surface free carriers excited by the probe light. However, in the lower-energy terahertz (THz) region, sensing by detecting molecular vibrations is still challenging because of low sensitivity, complicated spectral features, and relatively little accumulated knowledge of molecules. Here, we report the use of a micron-scale thin-slab metamaterial (MM) architecture, which functions as an amplifier for enhancing the absorption signal of the THz vibration of an ultrathin adsorbed layer of large organic molecules. We examined bovine serum albumin (BSA) as a prototype large protein molecule and Rhodamine 6G (Rh6G) and 3,3‧-diethylthiatricarbocyanine iodide (DTTCI) as examples of small molecules. Among them, our MM significantly magnified only the signal strength of bulky BSA. On the other hand, DTTCI and Rh6G are inactive, as they lack low-frequency vibrational modes in this frequency region. The results obtained here clearly demonstrate the promise of MM-enhanced absorption spectroscopy in the THz region for detection and structural monitoring of large biomolecules such as proteins or pathogenic enzymes.

  13. Pretreatment of oily samples for analysis by flow injection-spectrometric methods.

    Science.gov (United States)

    Burguera, José Luis; Burguera, Marcela

    2011-01-15

    This review presents a critical discussion of selected reports dealing with the pretreatment methods of oily samples and the determination of their organic and inorganic constituents using flow systems and spectrometric methods. Special emphasis is given to the on-line couplings with detection systems based on UV-visible spectrophotometry and spectrofluorimetry, atomic absorption spectrometry either with flame or electrothermal atomization as well as inductively coupled plasma optical emission spectrometry or inductively coupled plasma-mass spectrometry. Simple dilution with organic solvents, digestion with concentrated acids under thermal heating, microwave or ultrasound radiation and emulsification procedures are mostly used. The empirical preparation of certain organized assemblies like micelles, emulsions and specially microemulsions added to the confusion of some of the terms, demand a brief description of their characteristics, the correct formulation and some of their applications to the manipulation and treatment of oily samples. The analytical capabilities of combining flow manifolds with spectrometric methods for the determination of specific parameters in oily samples apparently have not been sufficiently exploited yet. PMID:21147308

  14. Infrared absorption of gaseous CH2BrOO detected with a step-scan Fourier-transform absorption spectrometer.

    Science.gov (United States)

    Huang, Yu-Hsuan; Lee, Yuan-Pern

    2014-10-28

    CH2BrOO radicals were produced upon irradiation, with an excimer laser at 248 nm, of a flowing mixture of CH2Br2 and O2. A step-scan Fourier-transform spectrometer coupled with a multipass absorption cell was employed to record temporally resolved infrared (IR) absorption spectra of reaction intermediates. Transient absorption with origins at 1276.1, 1088.3, 961.0, and 884.9 cm(-1) are assigned to ν4 (CH2-wagging), ν6 (O-O stretching), ν7 (CH2-rocking mixed with C-O stretching), and ν8 (C-O stretching mixed with CH2-rocking) modes of syn-CH2BrOO, respectively. The assignments were made according to the expected photochemistry and a comparison of observed vibrational wavenumbers, relative IR intensities, and rotational contours with those predicted with the B3LYP/aug-cc-pVTZ method. The rotational contours of ν7 and ν8 indicate that hot bands involving the torsional (ν12) mode are also present, with transitions 7(0)(1)12(v)(v) and 8(0)(1)12(v)(v), v = 1-10. The most intense band (ν4) of anti-CH2BrOO near 1277 cm(-1) might have a small contribution to the observed spectra. Our work provides information for directly probing gaseous CH2BrOO with IR spectroscopy, in either the atmosphere or laboratory experiments.

  15. Quantitative determination of α-ionone, β-ionone, and β-damascenone and enantiodifferentiation of α-ionone in wine for authenticity control using multidimensional gas chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Langen, Johannes; Wegmann-Herr, Pascal; Schmarr, Hans-Georg

    2016-09-01

    Native concentrations of α-ionone, β-ionone, and β-damascenone were studied in various authentic and commercial wines. In addition, the enantiomeric distribution of α-ionone was determined and its merits as a potential marker for aroma adulteration in wine were discussed. For extraction of volatiles, headspace solid-phase microextraction (HS-SPME) was applied, followed by heart-cut multidimensional gas chromatography coupled to tandem mass spectrometric detection for trace-level analysis. The enantioselective analysis of α-ionone was achieved with octakis(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin as the chiral selector in the separation column for gas chromatography (GC). In all the authentic wines studied, α-ionone showed a high enantiomeric ratio in favor of the (R)-enantiomer. Since an illegal addition of α-ionone in a racemic form changes the enantiomeric ratio, this ratio may serve as an adulteration marker. Concentrations varied between authenticity markers in wine. PMID:27417694

  16. Speciation and subcellular location of Se-containing proteins in human liver studied by sodium dodecyl sulfate-polyacrylamide gel electrophoresis and hydride generation-atomic fluorescence spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Chunying; Zhao, Jiujiang; Zhang, Peiqun; Chai, Zhifang [Institute of High Energy Physics and Laboratory of Nuclear Analytical Techniques, Chinese Academy of Sciences, Beijing (China)

    2002-02-01

    Speciation of Se-containing proteins in the subcellular fractions of human liver was studied by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) followed by hydride generation-atomic fluorescence spectrometric (HG-AFS) detection. It was found that about 24 kinds of Se-containing proteins existed in subcellular fractions of normal human liver. The molecular weights (MW) of the subunits were mostly in the range 20-30 kDa and 50-80 kDa. Major Se-containing protein fractions at 61 kDa and 21 kDa are probably selenoprotein P and glutathione peroxidase, respectively. The 54 kDa protein is probably a thioredoxin reductase, which is presented in nuclei, mitochondria, lysosome, microsome and cytosol. We noticed that the Se-containing protein with the lowest MW of 9.3 kDa only existed in lysosome. Most of the proteins have not been identified and would require further investigation to characterize them. The specific subcellular distributions of different Se-containing proteins suggest that they could play important biological roles in each organelle. (orig.)

  17. Quantitative determination of α-ionone, β-ionone, and β-damascenone and enantiodifferentiation of α-ionone in wine for authenticity control using multidimensional gas chromatography with tandem mass spectrometric detection.

    Science.gov (United States)

    Langen, Johannes; Wegmann-Herr, Pascal; Schmarr, Hans-Georg

    2016-09-01

    Native concentrations of α-ionone, β-ionone, and β-damascenone were studied in various authentic and commercial wines. In addition, the enantiomeric distribution of α-ionone was determined and its merits as a potential marker for aroma adulteration in wine were discussed. For extraction of volatiles, headspace solid-phase microextraction (HS-SPME) was applied, followed by heart-cut multidimensional gas chromatography coupled to tandem mass spectrometric detection for trace-level analysis. The enantioselective analysis of α-ionone was achieved with octakis(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin as the chiral selector in the separation column for gas chromatography (GC). In all the authentic wines studied, α-ionone showed a high enantiomeric ratio in favor of the (R)-enantiomer. Since an illegal addition of α-ionone in a racemic form changes the enantiomeric ratio, this ratio may serve as an adulteration marker. Concentrations varied between authenticity markers in wine.

  18. GMRT Detection of HI 21cm Associated Absorption towards the = 1.2 Red Quasar 3C 190

    Indian Academy of Sciences (India)

    C. H. Ishwara-Chandra; K. S. Dwarakanath; K. R. Anantharamaiah

    2003-03-01

    We report the GMRT detection of associated HI 21 cm-line absorption in the = 1.1946 red quasar 3C 190. Most of the absorption is blue-shifted with respect to the systemic redshift. The absorption, at ∼ 647.7MHz, is broad and complex, spanning a velocity width of ∼ 600 kms-1. Since the core is self-absorbed at this frequency, the absorption is most likely towards the hotspots. Comparison of the radio and deep optical images reveal linear filaments in the optical which overlap with the brighter radio jet towards the south-west.We therefore suggest that most of the HI 21 cm-line absorption could be occurring in the atomic gas shocked by the south-west jet.

  19. The Azimuthal Dependence of Outflows and Accretion Detected Using OVI Absorption

    CERN Document Server

    Kacprzak, Glenn G; Churchill, Christopher W; Nielsen, Nikole M; Charlton, Jane C

    2015-01-01

    We report a bimodality in the azimuthal angle ($\\Phi$) distribution of gas around galaxies traced by OVI absorption. We present the mean $\\Phi$ probability distribution function of 29 HST-imaged OVI absorbing (EW>0.1A) and 24~non-absorbing (EW<0.1A) isolated galaxies (0.08absorption is azimuthally dependent and occurs between $\\pm10-20^{\\circ}$ of the galaxy projected major axis and within $\\pm30^{\\circ}$ of the projected minor axis. We find higher EWs along the projected minor axis with weaker EWs along the project major axis. Highly inclined galaxies have the lowest covering fractions due to minimized outflow/inflow cross-section geometry. Absorbing galaxies also have bluer colors while non-absorbers have redder colors, suggesting that star-formation is a key driver in the OVI detection rate. OVI surrou...

  20. Invisible ink mark detection in the visible spectrum using absorption difference.

    Science.gov (United States)

    Lee, Joong; Kong, Seong G; Kang, Tae-Yi; Kim, Byounghyun; Jeon, Oc-Yeub

    2014-03-01

    One of popular techniques in gambling fraud involves the use of invisible ink marks printed on the back surface of playing cards. Such covert patterns are transparent in the visible spectrum and therefore invisible to unaided human eyes. Invisible patterns can be made visible with ultraviolet (UV) illumination or a CCD camera installed with an infrared (IR) filter depending on the type of ink materials used. Cheating gamers often wear contact lenses or eyeglasses made of IR or UV filters to recognize the secret marks on the playing cards. This paper presents an image processing technique to reveal invisible ink patterns in the visible spectrum without the aid of special equipment such as UV lighting or IR filters. A printed invisible ink pattern leaves a thin coating on the surface with different refractive index for different wavelengths of light, which results in color dispersion or absorption difference. The proposed method finds the differences of color components caused by absorption difference to detect invisible ink patterns on the surface. Experiment results show that the proposed scheme is effective for both UV-active and IR-active invisible ink materials. PMID:24529777

  1. Diffuse-light absorption spectroscopy by fiber optics for detecting and quantifying the adulteration of extra virgin olive oil

    Science.gov (United States)

    Mignani, A. G.; Ciaccheri, L.; Ottevaere, H.; Thienpont, H.; Conte, L.; Marega, M.; Cichelli, A.; Attilio, C.; Cimato, A.

    2010-09-01

    A fiber optic setup for diffuse-light absorption spectroscopy in the wide 400-1700 nm spectral range is experimented for detecting and quantifying the adulteration of extra virgin olive oil caused by lower-grade olive oils. Absorption measurements provide spectral fingerprints of authentic and adulterated oils. A multivariate processing of spectroscopic data is applied for discriminating the type of adulterant and for predicting its fraction.

  2. Combining asymmetrical flow field-flow fractionation with light-scattering and inductively coupled plasma mass spectrometric detection for characterization of nanoclay used in biopolymer nanocomposites

    DEFF Research Database (Denmark)

    Schmidt, Bjørn; Petersen, Jens Højslev; Koch, C. Bender;

    2009-01-01

    of clay nanoparticulates, an analytical system combining asymmetrical flow field-flow fractionation (AF4) with multi-angle light-scattering detection (MALS) and inductively coupled plasma mass spectrometry (ICP-MS) is presented. In a migration study, we tested a biopolymer nanocomposite consisting...

  3. Use of an oxidative destruction and quadrupole mass spectrometric (QMS) detection for the determination of the organic elemental composition of suspended matter in surface water

    NARCIS (Netherlands)

    Reijnders, H.F.R.; Onderdelinden, D.; Visser, M.G.; Griepink, B.

    1980-01-01

    A study was made of the applicability of a system consisting of a combustion followed by QMS-detection for the determination of the elemental composition of organic matter suspended in surface water. The solid material obtained from several types of water was collected by centrifugation. The results

  4. Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants

    NARCIS (Netherlands)

    Hankemeier, Th.; Rozenbrand, J.; Abhadur, M.; Vreuls, J.J.; Brinkman, U.A.Th.

    1998-01-01

    A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC system

  5. Speciation of selenoamino acids, selenonium ions and inorganic selenium by ion exchange HPLC with mass spectrometric detection and its application to yeast and algae

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Hansen, M.; Fan, T.;

    2001-01-01

    Cation and anion exchange HPLC were used to separate a mixture of 12 selenium species comprising selenoamino acids, selenonium ions and inorganic selenium. The cationic species were separated from each other and from the co-injected anions using a cation exchange column with gradient elution...... by aqueous pyridinium formate at pH similar to 3 as the mobile phase. The anionic species were separated using an anion exchange column with isocratic elution by an aqueous salicylate-TRIS mobile phase at pH 8.5. The separated selenium species were detected as Se-80 by ICP-dynamic reaction cell (DRC...... acid extract of Chlorella algae contained dimethylselenonium propionate (DMSeP), which was verified by HPLC-ES-MS. Se-allylselenocysteine and selenoethionine was detected at the low ng g(-1) concentration level based on co-chromatography with the standard substances spiked to the algal extract....

  6. Use of an oxidative destruction and quadrupole mass spectrometric (QMS) detection for the determination of the organic elemental composition of suspended matter in surface water

    OpenAIRE

    Reijnders, H.F.R.; Onderdelinden, D.; Visser, M.G.; Griepink, B.

    1980-01-01

    A study was made of the applicability of a system consisting of a combustion followed by QMS-detection for the determination of the elemental composition of organic matter suspended in surface water. The solid material obtained from several types of water was collected by centrifugation. The results show possible applications e.g. in the field of water characterization. A complete elemental analysis including pretreatment takes about 30 min.

  7. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection in the analysis of agrochemical residues and mycotoxins in food - challenges and applications.

    Science.gov (United States)

    O'Mahony, John; Clarke, Lesa; Whelan, Michelle; O'Kennedy, Richard; Lehotay, Steven J; Danaher, Martin

    2013-05-31

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence of UHPLC through technological advances. The implications of this new chromatographic technology for MS detection are discussed, as well as some of the remaining challenges in exploiting it for chemical residue applications. Finally, a comprehensive overview of published applications of UHPLC-MS in food contaminant analysis is presented, with a particular focus on veterinary drug residues.

  8. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    Four anionic and four cationic arsenic compounds in urine were separated by anion- and cation-exchange high-performance liquid chromatography and detected by inductively coupled plasma mass spectrometry (ICP-MS) at m/z 75. The species were the anions arsenite, arsenate, monomethylarsonate...... to arsenate in urine but was stable after at least 4-fold dilution of the urine with water. Arsenite was unstable in both urine samples and standard mixtures when diluted with the basic (pH 10.3) mobile phase used for anion chromatography. This could not be prevented by adding ascorbic acid as antioxidant...

  9. The use of ultra-high pressure liquid chromatography with tandem mass spectrometric detection in the analysis of agrochemical residues and mycotoxins in food - challenges and applications.

    Science.gov (United States)

    O'Mahony, John; Clarke, Lesa; Whelan, Michelle; O'Kennedy, Richard; Lehotay, Steven J; Danaher, Martin

    2013-05-31

    In the field of food contaminant analysis, the most significant development of recent years has been the integration of ultra-high pressure liquid chromatography (UHPLC), coupled to tandem quadrupole mass spectrometry (MS/MS), into analytical applications. In this review, we describe the emergence of UHPLC through technological advances. The implications of this new chromatographic technology for MS detection are discussed, as well as some of the remaining challenges in exploiting it for chemical residue applications. Finally, a comprehensive overview of published applications of UHPLC-MS in food contaminant analysis is presented, with a particular focus on veterinary drug residues. PMID:23352828

  10. Carbon nanotubes@silicon dioxide nanohybrids coating for solid-phase microextraction of organophosphorus pesticides followed by gas chromatography-corona discharge ion mobility spectrometric detection.

    Science.gov (United States)

    Saraji, Mohammad; Jafari, Mohammad Taghi; Mossaddegh, Mehdi

    2016-01-15

    A high efficiency solid-phase microextraction (SPME) fiber coated with porous carbon nanotubes-silicon dioxide (CNTs-SiO2) nanohybrids was synthesized and applied for the determination of some organophosphorus pesticides (OPPs) in vegetables, fruits and water samples. Gas chromatography-corona discharge ion mobility spectrometry was used as the detection system. Glucose, as a biocompatible compound, was used for connecting CNT and SiO2 during a hydrothermal process. The electrospinning technique was also applied for the fiber preparation. The parameters affecting the efficiency of extraction, including stirring rate, salt effect, extraction temperature, extraction time, desorption temperature and desorption time, were investigated and optimized. The developed CNTs@SiO2 fiber presented better extraction efficiency than the commercial SPME fibers (PA, PDMS, and PDMS-DVB). The intra- and inter-day relative standard deviations were found to be lower than 6.2 and 9.0%, respectively. For water samples, the limits of detection were in the range of 0.005-0.020 μg L(-1) and the limits of quantification were between 0.010 and 0.050 μg L(-1). The results showed a good linearity in the range of 0.01-3.0 μg L(-1) for the analytes. The spiking recoveries ranged from 79 (± 9) to 99 (± 8). The method was successfully applied for the determination of OPPs in real samples. PMID:26709024

  11. Flame atomic absorption spectrometric determination of zinc, nickel, iron and lead in different matrixes after solid phase extraction on sodium dodecyl sulfate (SDS)-coated alumina as their bis (2-hydroxyacetophenone)-1, 3-propanediimine chelates

    International Nuclear Information System (INIS)

    A sensitive and simple solid phase extraction method for the simultaneous determination of trace and toxic metals in food samples has been reported. The method is based on the adsorption of zinc, nickel, iron and lead on sodium dodecyl sulfate (SDS)-coated alumina, which is also chelated with bis (2-hydroxyacetophenone)-1, 3-propanediimine (BHAPN). The retained analyte ions on modified solid phase were eluted using 8 mL of 4 mol L-1 HNO3. The analyte determinations were carried out by flame atomic absorption spectrometry. The influences of some metal ions and anions on the recoveries of understudy analyte ions were investigated. The proposed method has been successfully applied for the evaluation of these trace and toxic metals in some traditional food samples from Iran.

  12. Main differences between volatiles of sparkling and base wines accessed through comprehensive two dimensional gas chromatography with time-of-flight mass spectrometric detection and chemometric tools.

    Science.gov (United States)

    Welke, Juliane Elisa; Zanus, Mauro; Lazzarotto, Marcelo; Pulgati, Fernando Hepp; Zini, Cláudia Alcaraz

    2014-12-01

    The main changes in the volatile profile of base wines and their corresponding sparkling wines produced by traditional method were evaluated and investigated for the first time using headspace solid-phase microextraction combined with comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry detection (GC×GC/TOFMS) and chemometric tools. Fisher ratios helped to find the 119 analytes that were responsible for the main differences between base and sparkling wines and principal component analysis explained 93.1% of the total variance related to the selected 78 compounds. It was also possible to observe five subclusters in base wines and four subclusters in sparkling wines samples through hierarchical cluster analysis, which seemed to have an organised distribution according to the regions where the wines came from. Twenty of the most important volatile compounds co-eluted with other components and separation of some of them was possible due to GC×GC/TOFMS performance.

  13. Mass-spectrometric identification of binding proteins of Mr 25,000 protein, a part of vitellogenin B1, detected in particulate fraction of Xenopus laevis oocytes.

    Science.gov (United States)

    Sugimoto, Isamu; Li, Zhijun; Yoshitome, Satoshi; Ito, Susumu; Hashimoto, Eikichi

    2004-10-01

    A phosphorylated protein with molecular mass of 25,000 (pp25) is a component of Xenopus laevis vitellogenin B1. Our previous report showed the existence of several binding proteins of pp25 in the particulate fraction of Xenopus oocytes. In an attempt to elucidate the function of pp25, two of these binding proteins were purified, analyzed by mass-spectrometry, and identified as ribosomal proteins S13 and S14. Other binding proteins in the particulate fraction mostly corresponded to those derived from purified 40S and 60S ribosomal subunits, as shown by the overlay assay method. However, pp25 did not show any effect on protein synthesis in the rabbit reticulocyte lysate system. A model in which pp25 connects a type of serpin (serine protease inhibitor), the only pp25-binding protein detected in the cytoplasm, to the endoplasmic reticulum through two serine clusters is proposed to explain a possible function of this protein.

  14. Standoff detection of bioaerosols over wide area using a newly developed sensor combining a cloud mapper and a spectrometric LIF lidar

    Science.gov (United States)

    Buteau, Sylvie; Simard, Jean-Robert; Roy, Gilles; Lahaie, Pierre; Nadeau, Denis; Mathieu, Pierre

    2013-10-01

    A standoff sensor called BioSense was developed to demonstrate the capacity to map, track and classify bioaerosol clouds from a distant range and over wide area. The concept of the system is based on a two steps dynamic surveillance: 1) cloud detection using an infrared (IR) scanning cloud mapper and 2) cloud classification based on a staring ultraviolet (UV) Laser Induced Fluorescence (LIF) interrogation. The system can be operated either in an automatic surveillance mode or using manual intervention. The automatic surveillance operation includes several steps: mission planning, sensor deployment, background monitoring, surveillance, cloud detection, classification and finally alarm generation based on the classification result. One of the main challenges is the classification step which relies on a spectrally resolved UV LIF signature library. The construction of this library relies currently on in-chamber releases of various materials that are simultaneously characterized with the standoff sensor and referenced with point sensors such as Aerodynamic Particle Sizer® (APS). The system was tested at three different locations in order to evaluate its capacity to operate in diverse types of surroundings and various environmental conditions. The system showed generally good performances even though the troubleshooting of the system was not completed before initiating the Test and Evaluation (T&E) process. The standoff system performances appeared to be highly dependent on the type of challenges, on the climatic conditions and on the period of day. The real-time results combined with the experience acquired during the 2012 T & E allowed to identify future ameliorations and investigation avenues.

  15. Herschel observations of Extra-Ordinary Sources (HEXOS) : Detection of hydrogen fluoride in absorption towards Orion KL

    NARCIS (Netherlands)

    Phillips, T. G.; Bergin, E. A.; Lis, D. C.; Neufeld, D. A.; Bell, T. A.; Wang, S.; Crockett, N. R.; Emprechtinger, M.; Blake, G.A.; Caux, E.; Ceccarelli, C.; Cernicharo, J.; Comito, C.; Daniel, F.; Dubernet, M. -L; Encrenaz, P.; Gerin, M.; Giesen, T. F.; Goicoechea, J. R.; Goldsmith, P. F.; Herbst, E.; Joblin, C.; Johnstone, D.; Langer, W. D.; Latter, W. D.; Lord, S. D.; Maret, S.; Martin, P. G.; Melnick, G. J.; Menten, K. M.; Morris, P.; Müller, H.S.P.; Murphy, J. A.; Ossenkopf, V.; Pearson, J. C.; Pérault, M.; Plume, R.; Qin, S.-L; Schilke, P.; Schlemmer, S.; Stutzki, J.; Trappe, N.; van der Tak, F. F. S.; Vastel, C.; Yorke, H. W.; Yu, S.; Zmuidzinas, J.; Boogert, A.; Güsten, R.; Hartogh, P.; Honingh, N.; Karpov, A.; Kooi, J.; Krieg, J. -M; Schieder, R.

    2010-01-01

    We report a detection of the fundamental rotational transition of hydrogen fluoride in absorption towards Orion KL using Herschel/HIFI. After the removal of contaminating features associated with common molecules (“weeds”), the HF spectrum shows a P-Cygni profile, with weak redshifted emission and s

  16. Detection of molecular absorption in the dayside of exoplanet 51 Pegasi b?

    CERN Document Server

    Brogi, M; de Kok, R J; Albrecht, S; Birkby, J L; de Mooij, E J W

    2013-01-01

    In this paper we present ground-based high-resolution spectroscopy of 51 Pegasi using CRIRES at the Very Large Telescope. The system was observed for 3x5 hours at 2.3 {\\mu}m at a spectral resolution of R = 100,000, targeting potential signatures from carbon monoxide, water vapour and methane in the planet's dayside spectrum. In the first 2x5 hours of data, we find a combined signal from carbon monoxide and water in absorption at a formal 5.9{\\sigma} confidence level, indicating a non-inverted atmosphere. We derive a planet mass of M_P = (0.46 +- 0.02) M_Jup and an orbital inclination i between 79.6 and 82.2 degrees, with the upper limit set by the non-detection of the planet transit in previous photometric monitoring. However, there is no trace of the signal in the final 5 hours of data. A statistical analysis indicates that the signal from the first two nights is robust, but we find no compelling explanation for its absence in the final night. The latter suffers from stronger noise residuals and greater inst...

  17. Detection of ocean glint and ozone absorption using LCROSS Earth observations

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, Tyler D. [NASA Ames Research Center, MS 245-3, Moffett Field, CA 94035 (United States); Ennico, Kimberly [NASA Ames Research Center, MS 245-6, Moffett Field, CA 94035 (United States); Meadows, Victoria S.; Sparks, William; Schwieterman, Edward W. [NASA Astrobiology Institute' s Virtual Planetary Laboratory, University of Washington, P.O. Box 351580, Seattle, WA 98195 (United States); Bussey, D. Ben J. [NASA Ames Research Center, MS 17-1, Moffett Field, CA 94089, USA Now the NASA Solar System Exploration Research Virtual Institute. (United States); Breiner, Jonathan, E-mail: tyler.d.robinson@nasa.gov [Astronomy Department, University of Washington, Seattle, WA 98195 (United States)

    2014-06-01

    The Lunar CRater Observation and Sensing Satellite (LCROSS) observed the distant Earth on three occasions in 2009. These data span a range of phase angles, including a rare crescent phase view. For each epoch, the satellite acquired near-infrared and mid-infrared full-disk images, and partial-disk spectra at 0.26-0.65 μm (λ/Δλ ∼ 500) and 1.17-2.48 μm (λ/Δλ ∼ 50). Spectra show strong absorption features due to water vapor and ozone, which is a biosignature gas. We perform a significant recalibration of the UV-visible spectra and provide the first comparison of high-resolution visible Earth spectra to the NASA Astrobiology Institute's Virtual Planetary Laboratory three-dimensional spectral Earth model. We find good agreement with the observations, reproducing the absolute brightness and dynamic range at all wavelengths for all observation epochs, thus validating the model to within the ∼10% data calibration uncertainty. Data-model comparisons reveal a strong ocean glint signature in the crescent phase data set, which is well matched by our model predictions throughout the observed wavelength range. This provides the first observational test of a technique that could be used to determine exoplanet habitability from disk-integrated observations at visible and near-infrared wavelengths, where the glint signal is strongest. We examine the detection of the ozone 255 nm Hartley and 400-700 nm Chappuis bands. While the Hartley band is the strongest ozone feature in Earth's spectrum, false positives for its detection could exist. Finally, we discuss the implications of these findings for future exoplanet characterization missions.

  18. Detection of ocean glint and ozone absorption using LCROSS Earth observations

    International Nuclear Information System (INIS)

    The Lunar CRater Observation and Sensing Satellite (LCROSS) observed the distant Earth on three occasions in 2009. These data span a range of phase angles, including a rare crescent phase view. For each epoch, the satellite acquired near-infrared and mid-infrared full-disk images, and partial-disk spectra at 0.26-0.65 μm (λ/Δλ ∼ 500) and 1.17-2.48 μm (λ/Δλ ∼ 50). Spectra show strong absorption features due to water vapor and ozone, which is a biosignature gas. We perform a significant recalibration of the UV-visible spectra and provide the first comparison of high-resolution visible Earth spectra to the NASA Astrobiology Institute's Virtual Planetary Laboratory three-dimensional spectral Earth model. We find good agreement with the observations, reproducing the absolute brightness and dynamic range at all wavelengths for all observation epochs, thus validating the model to within the ∼10% data calibration uncertainty. Data-model comparisons reveal a strong ocean glint signature in the crescent phase data set, which is well matched by our model predictions throughout the observed wavelength range. This provides the first observational test of a technique that could be used to determine exoplanet habitability from disk-integrated observations at visible and near-infrared wavelengths, where the glint signal is strongest. We examine the detection of the ozone 255 nm Hartley and 400-700 nm Chappuis bands. While the Hartley band is the strongest ozone feature in Earth's spectrum, false positives for its detection could exist. Finally, we discuss the implications of these findings for future exoplanet characterization missions.

  19. Detection of 21 Centimeter HI Absorption at z = 0.78 in a Survey of Radio Continuum Sources

    CERN Document Server

    Darling, J; Haynes, M P; Bolatto, A D; Bower, G C; Darling, Jeremy; Giovanelli, Riccardo; Haynes, Martha P.; Bolatto, Alberto D.; Bower, Geoffrey C.

    2004-01-01

    We report the detection of a deep broad HI 21 cm absorption system at z = 0.78 toward the radio source [HB89] 2351+456 (4C+45.51) at z = 1.992. The HI absorption was identified in a blind spectral line survey conducted at the Green Bank Telescope spanning 0.63 8.5 K, this system is by definition a damped Ly alpha absorption system (N(HI) >= 2 x 10^20 cm^-2). The line is unusually broad, with a FWHM of 53 km/s and a full span of 163 km/s, suggesting a physically extended HI gas structure. Radio surveys identify damped Ly alpha systems in a manner that bypasses many of the selection effects present in optical/UV surveys, including dust extinction and the atmospheric cutoff for z < 1.65. The smooth broad profile of this HI 21 cm absorption system is similar to the z = 0.89 HI absorption toward PKS 1830-211, which suggests that the absorber toward [HB89] 2351+456 is also a gravitational lens and a molecular absorption system. However, very long baseline interferometry and Hubble Space Telescope observations s...

  20. Detection of harmonics and recovery of the absorption line profile using logarithmic-transformed wavelength modulation spectroscopy

    Science.gov (United States)

    Cong, Menglong; Sun, Dandan

    2016-07-01

    A versatile signal processing strategy for eliminating the residual amplitude modulation (RAM) and distortion in tunable diode laser wavelength modulation spectroscopy is theoretically demonstrated and experimentally validated. The strategy involves logarithmic transformation and differential detection, which are achieved using a homemade circuit. Through the logarithmic transformation, the optical intensity modulation of the laser, which performs as the source of RAM and distortion, is separated from the absorption-induced power attenuation and further balanced during the differential detection. The first harmonic, which is proportional to the first-order derivative of the absorption line profile in the case of a small modulation index, is extracted along with the second harmonic and is integrated for the recovery of the absorption line profile. The experiments are carried out for CH4 at its R(3) absorption line of the 2ν3 overtone for validation of the system, and the derived results are found to be in good agreement with the theoretical simulations. These promising results indicate the high potential of the strategy for absorption spectrum-based determination of gas properties.

  1. Electrothermal atomic absorption spectrometric determination of vanadium in extracts of soil and sewage sludge certified reference materials after fractionation by means of the Communities Bureau of Reference modified sequential extraction procedure

    International Nuclear Information System (INIS)

    A modified three-step sequential extraction procedure proposed by the Commission of European Communities Bureau of Reference (BCR) was applied to certified reference materials of three different soil groups (rendzina, luvisol, cambisol) and sewage sludge of different composition originating from a municipal water treatment plant in order to assess potential mobility and the distribution of vanadium in the resulting fractions. Analysis of the extracts was carried out by electrothermal atomic absorption spectrometry with Zeeman background correction using transversely heated graphite atomizers. Extracts showed significant matrix interferences which were overcome by the standard addition technique. The original soil and sludge certified reference materials (CRMs) and the extraction residue from the sequential extraction were decomposed by a mixture of HNO3-HClO4-HF in an open system. The content of V determined after decomposition of the samples was in very good agreement with the certified total values. The accuracy of the sequential extraction procedure was checked by comparing the sum of the vanadium contents in the three fractions and in the extraction residue with the certified total content of V. The amounts of vanadium leached were in good correlation with the certified total contents of V in the CRMs of soils and sewage sludge. In the soils examined, vanadium was present almost entirely in the mineral lattice, while in the sewage sludge samples 9-14% was found in the oxidizable and almost 25% in the reducible fractions. The recovery ranged from 93-106% and the precision (RSD) was below 10%

  2. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  3. 分光光度计法快速检测果汁中嗜热耐酸菌%A Rapid Spectrometric Method for Detecting Alicyclobacillus acidoterrestris in Fruit Juice

    Institute of Scientific and Technical Information of China (English)

    叶建芳; 李文俊; 赵文超; 莫小晶; 贾彩凤

    2011-01-01

    酸土脂环酸芽孢杆菌(Alicyclobacillus acidoterrestris)是果汁污染的主要嗜酸耐热菌。它可以将香草酸或者香兰素转化为愈创木酚,后者在过氧化物酶的作用下产生红褐色产物,从而可以快速检测该菌。根据这个原理,设计实验探究该颜色反应的最优培养条件以及实际体系中检测该菌的可行性。结果表明:在静止培养情况下,在BAM培养基中添加100μg/kg的香草酸最有利于愈创木酚的产生;不同浓度的嗜热耐酸菌芽孢液在上述条件下培养,随着浓度的降低产生高浓度愈创木酚时间依次延迟,最低浓度为3个/mL的芽孢%In the presence of AlicyclobaciUus acidoterrestris, vanillic acid and vanillin can be converted into guaiacol, which can be further converted into a reddish-brown product by peroxidase. Based on this color reaction, a method was developed to spectrometrically detect the presence of Alicyclobacillus acidoterrestris in real systems. In static culture, BAM medium with the addition of 100 μg/kg vanillic acid was the most favorable for gualacol formation. The peak value of guaiacol concentration was delayed along with the decrease of bacteria concentration. A visible color was formed in medium and its OD470 could reach up to 1.0 or even more after 21 hours of culture at the initial spore density of 3 spores/mL. And the same result also was obtained in an apple juice system. Thus, this method can allow rapid, simple and sensitive detection ofAlicyclobacillus acidoterrestris in fruit juice.

  4. Herschel observations of EXtra-Ordinary Sources (HEXOS) : Detecting spiral arm clouds by CH absorption lines

    NARCIS (Netherlands)

    Qin, S.-L; Schilke, P.; Comito, C.; Möller, T.; Rolffs, R.; Müller, H.S.P.; Belloche, A.; Menten, K. M.; Lis, D. C.; Phillips, T. G.; Bergin, E. A.; Bell, T. A.; Crockett, N. R.; Blake, G.A.; Cabrit, S.; Caux, E.; Ceccarelli, C.; Cernicharo, J.; Daniel, F.; Dubernet, M. -L; Emprechtinger, M.; Encrenaz, P.; Falgarone, E.; Gerin, M.; Giesen, T. F.; Goicoechea, J. R.; Goldsmith, P. F.; Gupta, H.; Herbst, E.; Joblin, C.; Johnstone, D.; Langer, W. D.; Lord, S. D.; Maret, S.; Martin, P. G.; Melnick, G. J.; Morris, P.; Murphy, J. A.; Neufeld, D. A.; Ossenkopf, V.; Pagani, L.; Pearson, J. C.; Pérault, M.; Plume, R.; Salez, M.; Schlemmer, S.; Stutzki, J.; Trappe, N.; van der Tak, F. F. S.; Vastel, C.; Wang, S.; Yorke, H. W.; Yu, S.; Zmuidzinas, J.; Boogert, A.; Güsten, R.; Hartogh, P.; Honingh, N.; Karpov, A.; Kooi, J.; Krieg, J. -M; Schieder, R.; Diez-Gonzalez, M. C.; Bachiller, R.; Martin-Pintado, J.; Baechtold, W.; Olberg, M.; Nordh, L. H.; Gill, J. L.; Chattopadhyay, G.

    2010-01-01

    We have observed CH absorption lines (J = 3/2, N = 1 ≤ftarrow J = 1/2, N = 1) against the continuum source Sgr B2(M) using the Herschel/HIFI instrument. With the high spectral resolution and wide velocity coverage provided by HIFI, 31 CH absorption features with different radial velocities and line

  5. Stability of arsenic peptides in plant extracts: off-line versus on-line parallel elemental and molecular mass spectrometric detection for liquid chromatographic separation.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

    The instability of metal and metalloid complexes during analytical processes has always been an issue of an uncertainty regarding their speciation in plant extracts. Two different speciation protocols were compared regarding the analysis of arsenic phytochelatin (As(III)PC) complexes in fresh plant material. As the final step for separation/detection both methods used RP-HPLC simultaneously coupled to ICP-MS and ES-MS. However, one method was the often used off-line approach using two-dimensional separation, i.e. a pre-cleaning step using size-exclusion chromatography with subsequent fraction collection and freeze-drying prior to the analysis using RP-HPLC-ICP-MS and/or ES-MS. This approach revealed that less than 2% of the total arsenic was bound to peptides such as phytochelatins in the root extract of an arsenate exposed Thunbergia alata, whereas the direct on-line method showed that 83% of arsenic was bound to peptides, mainly as As(III)PC(3) and (GS)As(III)PC(2). Key analytical factors were identified which destabilise the As(III)PCs. The low pH of the mobile phase (0.1% formic acid) using RP-HPLC-ICP-MS/ES-MS stabilises the arsenic peptide complexes in the plant extract as well as the free peptide concentration, as shown by the kinetic disintegration study of the model compound As(III)(GS)(3) at pH 2.2 and 3.8. But only short half-lives of only a few hours were determined for the arsenic glutathione complex. Although As(III)PC(3) showed a ten times higher half-life (23 h) in a plant extract, the pre-cleaning step with subsequent fractionation in a mobile phase of pH 5.6 contributes to the destabilisation of the arsenic peptides in the off-line method. Furthermore, it was found that during a freeze-drying process more than 90% of an As(III)PC(3) complex and smaller free peptides such as PC(2) and PC(3) can be lost. Although the two-dimensional off-line method has been used successfully for other metal complexes, it is concluded here that the fractionation and

  6. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    Science.gov (United States)

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC. PMID:15910814

  7. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    Science.gov (United States)

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC.

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

    Science.gov (United States)

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-06-01

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

  9. Characterization of nuclear fuels by ICP mass-spectrometric techniques

    International Nuclear Information System (INIS)

    Isotopic analyses of radioactive materials such as irradiated nuclear fuel are of major importance for the optimization of the nuclear fuel cycle and for safeguard aspects. Among the mass-spectrometric techniques available, inductively coupled plasma mass spectrometry (ICP-MS) and thermal ionization mass spectrometry are the most frequently applied methods for nuclear applications. Because of the low detection limits, the ability to analyze the isotopic composition of the elements and the applicability of the techniques for measuring stable as well as radioactive nuclides with similar sensitivity, both mass-spectrometric techniques are an excellent amendment to classical radioactivity counting methods. The paper describes selected applications of multicollector ICP-MS in combination with chromatographic separation techniques and laser ablation for the isotopic analysis of irradiated nuclear fuels. The advantages and limitations of the selected analytical technique for the characterization of such a heterogeneous sample matrix are discussed. (orig.)

  10. A Nano-Biosensor for DNA Sequence Detection Using Absorption Spectra of SWNT-DNA Composite

    Directory of Open Access Journals (Sweden)

    J. Bansal

    2011-01-01

    Full Text Available A biosensor based on Single Walled Carbon Nanotube (SWNT-Poly (GTn ssDNA hybrid has been developed for medical diagnostics. The absorption spectrum of this assay is determined with the help of a Shimadzu UV-VIS-NIR spectrophotometer. Two distinct bands each containing three peaks corresponding to first and second van Hove singularities in the density of states of the nanotubes were observed in the absorption spectrum. When a single-stranded DNA (ssDNA having a sequence complementary to probic DNA is added to the ssDNA-SWNT conjugates, hybridization takes place, which causes the red shift of absorption spectrum of nanotubes. On the other hand, when the DNA is noncomplementary, no shift in the absorption spectrum occurs since hybridization between the DNA and probe does not take place. The red shifting of the spectrum is considered to be due to change in the dielectric environment around nanotubes.

  11. Detection of hydrogen fluoride absorption in diffuse molecular clouds with Herschel/HIFI: a ubiquitous tracer of molecular gas

    CERN Document Server

    Sonnentrucker, P; Phillips, T G; Gerin, M; Lis, D C; De Luca, M; Goicoechea, J R; Black, J H; Bell, T A; Boulanger, F; Cernicharo, J; Coutens, A; Dartois, E; Kazmierczak, M; Encrenaz, P; Falgarone, E; Geballe, T R; Giesen, T; Godard, B; Goldsmith, P F; Gry, C; Gupta, H; Hennebelle, P; Herbst, E; Hily-Blant, P; Joblin, C; Kolos, R; Krelowski, J; Mart\\in-Pintado, J; Menten, K M; Monje, R; Mookerjea, B; Pearson, J; Perault, M; Persson, C M; Plume, R; Salez, M; Schlemmer, S; Schmidt, M; Stutzki, J; Teyssier, D; Vastel, C; Yu, S; Caux, E; Gusten, R; Hatch, W A; Klein, T; Mehdi, I; Morris, P; Ward, J S

    2010-01-01

    We discuss the detection of absorption by interstellar hydrogen fluoride (HF) along the sight line to the submillimeter continuum sources W49N and W51. We have used Herschel's HIFI instrument in dual beam switch mode to observe the 1232.4762 GHz J = 1 - 0 HF transition in the upper sideband of the band 5a receiver. We detected foreground absorption by HF toward both sources over a wide range of velocities. Optically thin absorption components were detected on both sight lines, allowing us to measure - as opposed to obtain a lower limit on - the column density of HF for the first time. As in previous observations of HF toward the source G10.6-0.4, the derived HF column density is typically comparable to that of water vapor, even though the elemental abundance of oxygen is greater than that of fluorine by four orders of magnitude. We used the rather uncertain N(CH)-N(H2) relationship derived previously toward diffuse molecular clouds to infer the molecular hydrogen column density in the clouds exhibiting HF abs...

  12. Near-infrared diode laser based spectroscopic detection of ammonia: a comparative study of photoacoustic and direct optical absorption methods

    Science.gov (United States)

    Bozoki, Zoltan; Mohacsi, Arpad; Szabo, Gabor; Bor, Zsolt; Erdelyi, Miklos; Chen, Weidong; Tittel, Frank K.

    2002-01-01

    A photoacoustic spectroscopic (PAS) and a direct optical absorption spectroscopic (OAS) gas sensor, both using continuous-wave room-temperature diode lasers operating at 1531.8 nm, were compared on the basis of ammonia detection. Excellent linear correlation between the detector signals of the two systems was found. Although the physical properties and the mode of operation of both sensors were significantly different, their performances were found to be remarkably similar, with a sub-ppm level minimum detectable concentration of ammonia and a fast response time in the range of a few minutes.

  13. Can Ground-based Telescopes Detect The Oxygen 1.27 Micron Absorption Feature as a Biomarker in Exoplanets ?

    CERN Document Server

    Kawahara, Hajime; Takami, Michihiro; Fujii, Yuka; Kotani, Takayuki; Murakami, Naoshi; Tamura, Motohide; Guyon, Olivier

    2012-01-01

    The oxygen absorption line imprinted in the scattered light from the Earth-like planets has been considered as the most promising metabolic biomarker of the exo-life. We examine the feasibility of the detection of the oxygen 1.27 micron band from habitable exoplanets, in particular, around late-type stars with a 30 m class ground-based telescope with a future instrument. We analyzed the night airglow around 1.27 micron with IRCS/echelle spectrometer on Subaru and found that the strong telluric emission from atmospheric oxygen molecules declines by an order of magnitude by the midnight. With compilation of nearby star catalogues combined with the sky background model, we estimate the detectability of the oxygen absorption band from an Earth twin, if exists, around nearby stars. We find that the most dominant photon noise of the oxygen 1.27 micron detection comes from the night airglow if the leakage is suppressed enough to detect the planet. We conclude that the future detectors for which the detection contras...

  14. Herschel observations of extra-ordinary sources: Detection of Hydrogen Fluoride in absorption towards Orion~KL

    CERN Document Server

    Phillips, T G; Lis, D C; Neufeld, D A; Bell, T A; Wang, S; Crockett, N R; Emprechtinger, M; Blake, G A; Caux, E; Ceccarelli, C; Cernicharo, J; Comito, C; Daniel, F; Dubernet, M -L; Encrenaz, P; Gerin, M; Giesen, T F; Goicoechea, J R; Goldsmith, P F; Herbst, E; Joblin, C; Johnstone, D; Langer, W D; Latter, W D; Lord, S D; Maret, S; Martin, P G; Melnick, G J; Menten, K M; Morris, P; Muller, H S P; Murphy, J A; Ossenkopf, V; Pearson, J C; Perault, M; Plume, R; Qin, S -L; Schilke, P; Schlemmer, S; Stutzki, J; Trappe, N; van der Tak, F F S; Vastel, C; Yorke, H W; Yu, S; Zmuidzinas, J; Boogert, A; Gusten, R; Hartogh, P; Honingh, N; Karpov, A; Kooi, J; Krieg, J -M; Schieder, R

    2010-01-01

    We report a detection of the fundamental rotational transition of hydrogen fluoride in absorption towards Orion KL using Herschel/HIFI. After the removal of contaminating features associated with common molecules ("weeds"), the HF spectrum shows a P-Cygni profile, with weak redshifted emission and strong blue-shifted absorption, associated with the low-velocity molecular outflow. We derive an estimate of 2.9 x 10^13 cm^-2 for the HF column density responsible for the broad absorption component. Using our best estimate of the H2 column density within the low-velocity molecular outflow, we obtain a lower limit of ~1.6 x 10^-10 for the HF abundance relative to hydrogen nuclei, corresponding to 0.6% of the solar abundance of fluorine. This value is close to that inferred from previous ISO observations of HF J=2--1 absorption towards Sgr B2, but is in sharp contrast to the lower limit of 6 x 10^-9 derived by Neufeld et al. (2010) for cold, foreground clouds on the line of sight towards G10.6-0.4.

  15. HST hot Jupiter Transmission Spectral Survey: A detection of Na and strong optical absorption in HAT-P-1b

    CERN Document Server

    Nikolov, N; Pont, F; Burrows, A S; Fortney, J J; Ballester, G E; Evans, T M; Huitson, C M; Wakeford, H R; Wilson, P A; Aigrain, S; Deming, D; Gibson, N P; Henry, G W; Knutson, H; Etangs, A Lecavelier des; Showman, A P; Vidal-Madjar, A; Zahnle, K

    2013-01-01

    We present an optical to near-infrared transmission spectrum of the hot Jupiter HAT-P-1b, based on HST observations, covering the spectral regime from 0.29 to 1.027{\\mu}m with STIS, which is coupled with a recent WFC3 transit (1.087 to 1.687{\\mu}m). We derive refined physical parameters of the HAT-P-1 system, including an improved orbital ephemeris. The transmission spectrum shows a strong absorption signature shortward of 0.55{\\mu}m, with a strong blueward slope into the near-ultraviolet. We detect atmospheric sodium absorption at a 3.3{\\sigma} significance level, but find no evidence for the potassium feature. The red data implies a marginally flat spectrum with a tentative absorption enhancement at wavelength longer than ~0.85{\\mu}m. The STIS and WFC3 spectra differ significantly in absolute radius level (4.3 +/- 1.6 pressure scale heights), implying strong optical absorption in the atmosphere of HAT-P-1b. The optical to near-infrared difference cannot be explained by stellar activity, as simulta- neous st...

  16. Mass Spectrometric Method for Analyzing Metabolites in Yeast with Single Cell Sensitivity

    NARCIS (Netherlands)

    Amantonico, Andrea; Oh, Joo Yeon; Sobek, Jens; Heinemann, Matthias; Zenobi, Renato

    2008-01-01

    Getting a look-in: An optimized MALDI-MS procedure has been developed to detect endogenous primary metabolites directly in the cell extract. A detection limit corresponding to metabolites from less than a single cell has been attained, opening the door to single-cell metabolomics by mass spectrometr

  17. Detection of hydrogen peroxide based on long-path absorption spectroscopy using a CW EC-QCL

    Science.gov (United States)

    Sanchez, N. P.; Yu, Y.; Dong, L.; Griffin, R.; Tittel, F. K.

    2016-02-01

    A sensor system based on a CW EC-QCL (mode-hop-free range 1225-1285 cm-1) coupled with long-path absorption spectroscopy was developed for the monitoring of gas-phase hydrogen peroxide (H2O2) using an interference-free absorption line located at 1234.055 cm-1. Wavelength modulation spectroscopy (WMS) with second harmonic detection was implemented for data processing. Optimum levels of pressure and modulation amplitude of the sensor system led to a minimum detection limit (MDL) of 25 ppb using an integration time of 280 sec. The selected absorption line for H2O2, which exhibits no interference from H2O, makes this sensor system suitable for sensitive and selective monitoring of H2O2 levels in decontamination and sterilization processes based on Vapor Phase Hydrogen Peroxide (VPHP) units, in which a mixture of H2O and H2O2 is generated. Furthermore, continuous realtime monitoring of H2O2 concentrations in industrial facilities employing this species can be achieved with this sensing system in order to evaluate average permissible exposure levels (PELs) and potential exceedances of guidelines established by the US Occupational Safety and Health Administration for H2O2.

  18. Inability to detect significant absorption of immunoreactive soya protein in healthy adults may be relevant to its weak allergenicity

    DEFF Research Database (Denmark)

    Lund, Cecilia M; Dirks, Christina G; Pedersen, Mona H;

    2013-01-01

    ABSTRACT: Soya and peanut are botanically closely related and share cross-reacting antigens, but compared to soya, peanut allergy has a higher prevalence with more severe allergic reactions. Furthermore, the threshold dose for eliciting reactions is higher for soya. A difference in undigested...... protein absorption between the two foods, might explain this diversity.In the current study the amount of soya protein absorbed after soya bean ingestion in healthy adults was estimated. Ten subjects ingested 100 grams of soya beans (40 grams of soya protein) and blood was drawn before and 1, 3 and 24...... hours after administration. Serum was analysed by ELISA and histamine release (HR). In all serum samples the soya protein concentration was below quantification limit (1.6 ng/ml which corresponds to 4.8 mug or 0.12 parts per million absorbed soya protein.We could not detect any significant absorption...

  19. The physical understanding on dynamic readout/detection of super-resolution pits with nonlinear reverse saturation absorption thin films

    International Nuclear Information System (INIS)

    The physical mechanism and understanding behind dynamic readout/detection of super-resolution pits with a nonlinear reverse-saturation absorption active layer, such as an InSb active layer, is presented on the basis of experimental results of open-aperture z-scan measurements and pump–probe transient time response analysis. The super-resolution of an InSb active layer is a result of the formation of a sub-wavelength scatterer region at the center of the focused spot. The frequency response function also verifies that the cutoff frequency with an InSb active layer is clearly extended compared to when an InSb active layer is not used. The findings are useful for understanding the physical process of the far-field super-resolution effect with nonlinear reverse-saturation absorption characteristics. (paper)

  20. Highly Selective Hg (II Ion Detection Based on Linear Blue-Shift of the Maximum Absorption Wavelength of Silver Nanoparticles

    Directory of Open Access Journals (Sweden)

    Li Ping Wu

    2012-01-01

    Full Text Available A new method of detecting Hg (II ion with silver nanoparticles (AgNPs is developed in this contribution. When Hg (II ions were added into AgNPs solution, the solution displayed rapid color change and blue shift of the maximum absorption wavelength (Δλ, which was in proportion to the Hg (II ion concentration over the range of 2.0 × 10−7–6.0 × 10−6 mol/L, with detection limit (3σ of 6.6 × 10−9 mol/L. Under the same experimental conditions, other metal ions did not interfere. Thus, we propose a rapid, simple and highly selective method for detecting Hg (II ion.

  1. A survey for HI in the distant Universe: the detection of associated 21-cm absorption at z=1.28

    CERN Document Server

    Curran, S J; Tanna, A; Sadler, E M; Pracy, M B; Athreya, R

    2012-01-01

    We have undertaken a survey for HI 21-cm absorption within the host galaxies of z ~ 1.2 - 1.5 radio sources, in the search of the cool neutral gas currently "missing" at z > 1. This deficit is believed to be due to the optical selection of high redshift objects biasing surveys towards sources of sufficient ultra-violet luminosity to ionise all of the gas in the surrounding galaxy. In order to avoid this bias, we have selected objects above blue magnitudes of B\\sim20, indicating ultra-violet luminosities below the critical value above which 21-cm has never been detected. As a secondary requirement to the radio flux and faint optical magnitude, we shortlist targets with radio spectra suggestive of compact sources, in order to maximise the coverage of background emission. From this, we obtain one detection out of ten sources searched, which at z=1.278 is the third highest redshift detection of associated 21-cm absorption to date. Accounting for the spectra compromised by radio frequency interference, as well as ...

  2. Determination of Pb(Ⅱ) and Cu(Ⅱ) by Electrothermal Atomic Absorption Spectrometry after Preconcentration by a Schiff Base Adsorbed on Surfactant Coated Alumina

    Institute of Scientific and Technical Information of China (English)

    SABER TEHRANI Mohammad; RASTEGAR Faramarz; PARCHEHBAF Ayob; KHATAMIAN Masoomeh

    2006-01-01

    1,2-Bis(salicylidenamino)ethane loaded onto sodium dodecyl sulfate-coated alumina was used as a new chelating sorbent for the preconcentration of traces of Pb(Ⅱ) and Cu(Ⅱ) prior to atomic absorption spectrometric determination. The influence of pH, flow rates of sample and eluent solutions, and foreign ions on the recovery of Pb(Ⅱ)by electrothermal atomic absorption spectrometry (ETAAS). The data of limit of detection (3σ) for Pb(Ⅱ) and Cu(Ⅱ)posed method was successfully applied to determination of lead and copper in different water samples.

  3. Changing of Bacteria Catalase Activity Under the Influence of Electro-Magnetic Radiation on a Frequency of Nitric Oxide Absorption and Radiation Molecular Spectrum

    Directory of Open Access Journals (Sweden)

    G.M. Shub

    2009-09-01

    Full Text Available The dynamics of catalase activity degree changing in Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa is described under the influence of electro-magnetic radiation on a frequency of nitric oxide absorption and radiation molecular spectrum. The panoramic spectrometric measuring complex, developed in Central Scientific Research Institute of measuring equipment Public corporation, Saratov, was used while carrying out the research. Electromagnetic vibrations of extremely high frequencies were stimulated in this complex imitating the structure of nitric oxide absorption and radiation molecular spectrum. The growth of activity of the mentioned enzyme of the strains under research was detected. The most significant changes were observed under 60-minutes exposure.

  4. Accuracy of X-ray fluorescence spectrometric determination of Rb and Sr concentrations in rock samples

    International Nuclear Information System (INIS)

    It is shown that application of the Compton scattering for matrix correction in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide concentrations at a relative accuracy level of 1%. The empirical method applies to rock samples showing differences in mass absorption up to a factor of two. The accuracy of the method has been tested by analysis of 57 samples analysed for Rb and Sr by mass spectrometric isotope dilution. In addition a few of the U.S. Geological Survey reference rock powders, showing significantly different mass absorption, were analysed for Rb and Sr. It is demonstrated that the mica effect, if significant, is smaller than 1% relative. There is no advantage in the use of the LiF(220) analysing crystal as a substitute for the LiF(200). The method appears to be insensitive to the pellet thickness. (author)

  5. A carbon monoxide detection device based on mid-infrared absorption spectroscopy at 4.6 μm

    Science.gov (United States)

    Li, Guo-Lin; Sui, Yue; Dong, Ming; Ye, Wei-Lin; Zheng, Chuan-Tao; Wang, Yi-Ding

    2015-05-01

    We present a differential carbon monoxide (CO) concentration sensing device using a self-fabricated spherical mirror (e.g., light collector) and a multi-pass gas chamber. Single-source dual-channel detection method is adopted to suppress the interferences from light source, optical path, and environmental changes. The detection principle of the device is described, and both the optical part and the electrical part are designed and developed. Experiments are carried out to evaluate the sensing performances on CO concentration. The results indicate that the limit of detection is about 10 ppm with an absorption length of 40 cm. As the gas concentration gets larger than 100 ppm, the relative detection error falls into the range of -1.7 to +1.9 %. Based on 12-h long-term measurements on the 100 and 1000 ppm CO samples, the maximum detection errors are about 0.9 and 5.5 %, respectively. Benefit from low cost and competitive characteristics, the proposed device shows potential applications in CO detection under the circumstances of coal-mine production and environmental protection.

  6. Reversed phase and cation exchange liquid chromatography with spectrophotometric and elemental/molecular mass spectrometric detection for S-adenosyl methionine/S-adenosyl homocysteine ratios as methylation index in cell cultures of ovarian cancer.

    Science.gov (United States)

    Iglesias González, T; Cinti, M; Montes-Bayón, M; Fernández de la Campa, M R; Blanco-González, E

    2015-05-01

    S-adenosylmethionine (SAM) and S-adenosylhomocysteine (SAH) are essential compounds in the carbon metabolic cycle that have clinical implications in a broad range of disease conditions. The measurement of the ratio SAM/SAH also called methylation index, has become a way of monitoring the DNA methylation of a cell which is an epigenetic event with important clinical implications in diagnosis; therefore the development of suitable methods to accurately quantify these compounds is mandatory. This work illustrates the comparison of three independent methods for the determination of the methylation index, all of them based on the chromatographic separation of the two species (SAM and SAH) using either ion-pairing reversed phase or cation exchange chromatography. The species detection was conducted using either molecular absorption spectrophotometry (HPLC-UV) or mass spectrometry with electrospray (ESI-MS/MS) as ionization source or inductively coupled plasma (DF-ICP-MS) by monitoring the S-atom contained in both analytes. The analytical performance characteristics of the three methods were critically compared obtaining best features for the combination of reversed phase HPLC with ESI-MS in the MRM mode. In this case, detection limits of about 0.5ngmL(-1) for both targeted analytes permitted the application of the designed strategy to evaluate the effect of cisplatin on the changes of the methylation index among epithelial ovarian cancer cell lines sensitive (A2780) and resistant (A2780CIS) to this drug after exposition to cisplatin.

  7. Invisible Active Galactic Nuclei. II Radio Morphologies & Five New HI 21 cm Absorption Line Detections

    OpenAIRE

    Yan, Ting; Stocke, John T.; Darling, Jeremy; Momjian, Emmanuel; Sharma, Soniya; Kanekar, Nissim

    2015-01-01

    We have selected a sample of 80 candidates for obscured radio-loud active galactic nuclei and presented their basic optical/near-infrared (NIR) properties in Paper 1. In this paper, we present both high-resolution radio continuum images for all of these sources and HI 21cm absorption spectroscopy for a few selected sources in this sample. A-configuration 4.9 and 8.5 GHz VLA continuum observations find that 52 sources are compact or have substantial compact components with size

  8. Photometric and emission-spectrometric determination of boron in steels

    International Nuclear Information System (INIS)

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated. (orig.)

  9. Photometric and emission-spectrometric determination of boron in steels

    Energy Technology Data Exchange (ETDEWEB)

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated.

  10. Aspects of optical fibers and spectrometric sensors in chemical process and industrial environments

    International Nuclear Information System (INIS)

    For on-line control, the two alternatives of automatic sample transfer and in situ remote analysis are discussed. New concepts are emerging from the possibilities offered by optical fibers. Absorption in the visible, UV and IR, fluorescence and Raman spectrometric techniques are examined. The state of the art of optodes and devices in chemical process control are given, with some examples of applications in nuclear plants

  11. The detection of carbon dioxide leaks using quasi-tomographic laser absorption spectroscopy measurements in variable wind

    Directory of Open Access Journals (Sweden)

    Z. H. Levine

    2015-11-01

    Full Text Available Laser Absorption Spectroscopy (LAS has been used over the last several decades for the measurement of trace gasses in the atmosphere. For over a decade, LAS measurements from multiple sources and tens of retroreflectors have been combined with sparse-sample tomography methods to estimate the 2-D distribution of trace gas concentrations and underlying fluxes from pointlike sources. In this work, we consider the ability of such a system to detect and estimate the position and rate of a single point leak which may arise as a failure mode for carbon dioxide storage. The leak is assumed to be at a constant rate giving rise to a plume with a concentration and distribution that depend on the wind velocity. We demonstrate the ability of our approach to detect a leak using numerical simulation and a preliminary measurement.

  12. Detection Limit of Glucose Concentration with Near-Infrared Absorption and Scattering Spectroscopy

    Institute of Scientific and Technical Information of China (English)

    LUO Yun-Han; HUANG Fu-Rong; LI Shi-Ping; CHEN Zhe

    2008-01-01

    @@ Theoretical analyses and Monte Carlo simulation are performed to investigate the detection limit of glucose concentration with near-infrared spectroscopy.The relation between detection limitation of glucose concentration and source-detector separation is derived.Monte Carlo simulation performed with a skin-layered model shows that the ratio of effective photons from the target layer could excess 50% by selecting proper source-detector separation,and that the detection limit of glucose concentration approaches to 0.28mM,which satisfies the requirement of food and drug administration for noninvasive glucose sensing.

  13. Protein nitration in biological aging: proteomic and tandem mass spectrometric characterization of nitrated sites.

    Science.gov (United States)

    Kanski, Jaroslaw; Schöneich, Christian

    2005-01-01

    Proteomic techniques for the identification of 3-nitrotyrosine-containing proteins in various biological systems are described with emphasis on the direct mass spectrometric detection and sequencing of 3-nitrotyrosine-containing peptides. Strengths and weaknesses of various separation and mass spectrometric techniques are discussed. Some examples for the MS/MS analysis of nitrated peptides obtained from aging rat heart and skeletal muscle are provided, such as nitration of Tyr105 of the mitochondrial electron-transfer flavoprotein and Tyr14 of creatine kinase.

  14. Significance of Airborne Gamma-ray spectrometric data of Umm bisilla Area, central Eastern Desert, Egypt

    International Nuclear Information System (INIS)

    Umm bisilla area, located in the Central Eastern Desert of Egypt, consists mainly of basement rocks. The present investigation of the airborne spectrometric data is to define the meaningful anomalies from the raw data by applying the significance factor techniques, by calculating the significant radioactive provinces. Determination of the gross structural pattern and broad variations in composition of the crystalline basement, to define the relationships between the tectonic features of the area as interpreted from aeromagnetic data, with the significant anomalies revealed from spectrometric data was carried out through the application of different magnetic techniques. Five significant uraniferous zones were detected associated with Umm Bisilla granite, amphibolite, and grey granite. The intersection of the structural lineaments interpreted from aeromagnetic data illustrated good correlation with the significant uranium anomalous zones interpreted from spectrometric data, and indicated that the concentration is structurally. 15 figs

  15. X-ray spectrometric determination of thorium in bone and other biological materials

    International Nuclear Information System (INIS)

    An x-ray spectrometric method has been developed for the determination of thorium in bone and other biological materials. The limit of detection at the 95% confidence level is 20 ng. This corresponds to a concentration of 2 ppb in a 10-g sample of bone ash

  16. QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods

    Science.gov (United States)

    This chapter describes an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in foods using gas and/or liquid chromatographic (GC and/or LC) analytical separation and mass spectrometric (MS) detection. The approach is known as QuEChERS, which stands fo...

  17. 'Intelligent' triggering methodology for improved detectability of wavelength modulation diode laser absorption spectrometry applied to window-equipped graphite furnaces

    International Nuclear Information System (INIS)

    The wavelength modulation-diode laser absorption spectrometry (WM-DLAS) technique experiences a limited detectability when window-equipped sample compartments are used because of multiple reflections between components in the optical system (so-called etalon effects). The problem is particularly severe when the technique is used with a window-equipped graphite furnace (GF) as atomizer since the heating of the furnace induces drifts of the thickness of the windows and thereby also of the background signals. This paper presents a new detection methodology for WM-DLAS applied to a window-equipped GF in which the influence of the background signals from the windows is significantly reduced. The new technique, which is based upon a finding that the WM-DLAS background signals from a window-equipped GF are reproducible over a considerable period of time, consists of a novel 'intelligent' triggering procedure in which the GF is triggered at a user-chosen 'position' in the reproducible drift-cycle of the WM-DLAS background signal. The new methodology makes also use of 'higher-than-normal' detection harmonics, i.e. 4f or 6f, since these previously have shown to have a higher signal-to-background ratio than 2f-detection when the background signals originates from thin etalons. The results show that this new combined background-drift-reducing methodology improves the limit of detection of the WM-DLAS technique used with a window-equipped GF by several orders of magnitude as compared to ordinary 2f-detection, resulting in a limit of detection for a window-equipped GF that is similar to that of an open GF

  18. Spectrometric mixture analysis: An unexpected wrinkle

    Indian Academy of Sciences (India)

    Robert De Levie

    2009-09-01

    The spectrometric analysis of a mixture of two chemically and spectroscopically similar compounds is illustrated for the simultaneous spectrometric determination of caffeine and theobromine, the primary stimulants in coffee and tea, based on their ultraviolet absorbances. Their analysis indicates that such measurements may need an unexpectedly high precision to yield accurate answers, because of an artifact of inverse cancellation, in which a small noise or drift signal is misinterpreted in terms of a concentration difference. The computed sum of the concentrations is not affected.

  19. Detection of Ocean Glint and Ozone Absorption Using LCROSS Earth Observations

    CERN Document Server

    Robinson, Tyler D; Meadows, Victoria S; Sparks, William; Bussey, D Ben J; Schwieterman, Edward W; Breiner, Jonathan

    2014-01-01

    The Lunar CRater Observation and Sensing Satellite (LCROSS) observed the distant Earth on three occasions in 2009. These data span a range of phase angles, including a rare crescent phase view. For each epoch, the satellite acquired near-infrared and mid-infrared full-disk images, and partial-disk spectra at 0.26-0.65 microns (R~500) and 1.17-2.48 microns (R~50). Spectra show strong absorption features due to water vapor and ozone, which is a biosignature gas. We perform a significant recalibration of the UV-visible spectra and provide the first comparison of high-resolution visible Earth spectra to the NASA Astrobiology Institute's Virtual Planetary Laboratory three-dimensional spectral Earth model. We find good agreement with the observations, reproducing the absolute brightness and dynamic range at all wavelengths for all observation epochs, thus validating the model to within the ~10% data calibration uncertainty. Data-model comparisons reveal a strong ocean glint signature in the crescent phase dataset, ...

  20. Cavity enhanced absorption spectroscopy for N2O detection at 2.86μm using a continuous tunable color center laser

    Institute of Scientific and Technical Information of China (English)

    Shaocheng Li(李少成); Qingxu Yu(于清旭); Maarten van Herpen; Sacco te Lintel Hekkert; Frans J. M. Harren

    2003-01-01

    The cavity enhanced absorption technique is applied to N2O detection around 2.86 μm using a continuouswave color center laser. A high-finesse triangular ring cavity is used in this technology. Transmission through the cavity is obtained by jittering the cavity-length with a piezo on one of the cavity mirrors.A minimum detectable absorption coefficient of 2 × 10-6 cm-1 is achieved with a mirror reflectivity of 99.24%, corresponding to a N2O detection limit of 600 parts per billion.

  1. Ion chromatography with the indirect ultraviolet detection of alkali metal ions and ammonium using imidazolium ionic liquid as ultraviolet absorption reagent and eluent.

    Science.gov (United States)

    Liu, Yong-Qiang; Yu, Hong

    2016-08-01

    Indirect ultraviolet detection was conducted in ultraviolet-absorption-agent-added mobile phase to complete the detection of the absence of ultraviolet absorption functional group in analytes. Compared with precolumn derivatization or postcolumn derivatization, this method can be widely used, has the advantages of simple operation and good linear relationship. Chromatographic separation of Li(+) , Na(+) , K(+) , and NH4 (+) was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid/organic solvent as the mobile phase, in which imidazolium ionic liquids acted as ultraviolet absorption reagent and eluting agent. The retention behaviors of four kinds of cations are discussed, and the mechanism of separation and detection are described. The main factors influencing the separation and detection were the background ultraviolet absorption reagent and the concentration of hydrogen ion in the ion chromatography-indirect ultraviolet detection. The successful separation and detection of Li(+) , Na(+) , K(+) , and NH4 (+) within 13 min was achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.02, 0.11, 0.30, and 0.06 mg/L, respectively. A new separation and analysis method of alkali metal ions and ammonium by ion chromatography with indirect ultraviolet detection method was developed, and the application range of ionic liquid was expanded.

  2. Detecting Newcastle disease virus in combination of RT-PCR with red blood cell absorption

    Directory of Open Access Journals (Sweden)

    Liu Chengqian

    2011-05-01

    Full Text Available Abstract Reverse transcription-polymerase chain reaction (RT-PCR has limited sensitivity when treating complicated samples, such as feces, waste-water in farms, and nucleic acids, protein rich tissue samples, all the factors may interfere with the sensitivity of PCR test or generate false results. In this study, we developed a sensitive RT-PCR, combination of red blood cell adsorption, for detecting Newcastle disease virus (NDV. One pair of primers which was highly homologous to three NDV pathotypes was designed according to the consensus nucleocapsid protein (NP gene sequence. To eliminate the interfere of microbes and toxic substances, we concentrated and purified NDV from varied samples utilizing the ability of NDV binding red blood cells (RBCs. The RT-PCR coupled with red blood cell adsorption was much more sensitive in comparison with regular RT-PCR. The approach could also be used to detect other viruses with the property of hemagglutination, such as influenza viruses.

  3. Multilayer Cloud Detection with the MODIS Near-Infrared Water Vapor Absorption Band

    Science.gov (United States)

    Wind, Galina; Platnick, Steven; King, Michael D.; Hubanks, Paul A,; Pavolonis, Michael J.; Heidinger, Andrew K.; Yang, Ping; Baum, Bryan A.

    2009-01-01

    Data Collection 5 processing for the Moderate Resolution Imaging Spectroradiometer (MODIS) onboard the NASA Earth Observing System EOS Terra and Aqua spacecraft includes an algorithm for detecting multilayered clouds in daytime. The main objective of this algorithm is to detect multilayered cloud scenes, specifically optically thin ice cloud overlying a lower-level water cloud, that presents difficulties for retrieving cloud effective radius using single layer plane-parallel cloud models. The algorithm uses the MODIS 0.94 micron water vapor band along with CO2 bands to obtain two above-cloud precipitable water retrievals, the difference of which, in conjunction with additional tests, provides a map of where multilayered clouds might potentially exist. The presence of a multilayered cloud results in a large difference in retrievals of above-cloud properties between the CO2 and the 0.94 micron methods. In this paper the MODIS multilayered cloud algorithm is described, results of using the algorithm over example scenes are shown, and global statistics for multilayered clouds as observed by MODIS are discussed. A theoretical study of the algorithm behavior for simulated multilayered clouds is also given. Results are compared to two other comparable passive imager methods. A set of standard cloudy atmospheric profiles developed during the course of this investigation is also presented. The results lead to the conclusion that the MODIS multilayer cloud detection algorithm has some skill in identifying multilayered clouds with different thermodynamic phases

  4. Detection of gastrointestinal cancer by elastic scattering and absorption spectroscopies with the Los Alamos Optical Biopsy System

    Energy Technology Data Exchange (ETDEWEB)

    Mourant, J.R.; Boyer, J.; Johnson, T.M.; Lacey, J.; Bigio, I.J. [Los Alamos National Lab., NM (United States); Bohorfoush, A. [Wisconsin Medical School, Milwaukee, WI (United States). Dept. of Gastroenterology; Mellow, M. [Univ. of Oklahoma Medical School, Oklahoma City, OK (United States). Dept. of Gastroenterology

    1995-03-01

    The Los Alamos National Laboratory has continued the development of the Optical Biopsy System (OBS) for noninvasive, real-time in situ diagnosis of tissue pathologies. In proceedings of earlier SPIE conferences we reported on clinical measurements in the bladder, and we report here on recent results of clinical tests in the gastrointestinal tract. With the OBS, tissue pathologies are detected/diagnosed using spectral measurements of the elastic optical transport properties (scattering and absorption) of the tissue over a wide range of wavelengths. The use of elastic scattering as the key to optical tissue diagnostics in the OBS is based on the fact that many tissue pathologies, including a majority of cancer forms, exhibit significant architectural changes at the cellular and sub-cellular level. Since the cellular components that cause elastic scattering have dimensions typically on the order of visible to near-IR wavelengths, the elastic (Mie) scattering properties will be wavelength dependent. Thus, morphology and size changes can be expected to cause significant changes m an optical signature that is derived from the wavelength-dependence of elastic scattering. Additionally, the optical geometry of the OBS beneficially enhances its sensitivity for measuring absorption bands. The OBS employs a small fiber-optic probe that is amenable to use with any endoscope or catheter, or to direct surface examination, as well as interstitial needle insertion. Data acquistion/display time is <1 second.

  5. On the Putative Detection of z>0 X-ray Absorption Features in the Spectrum of Markarian 421

    CERN Document Server

    Rasmussen, A P; Den Herder, J W A; Kaastra, J; Kahn, S M; Paerels, F; Herder, Jan Willem den; Kaastra, Jelle; Kahn, Steven M.; Paerels, Frits; Rasmussen, Andrew P.; Vries, Cor de

    2006-01-01

    In a series of papers, Nicastro et al. have claimed the detection of z>0 O VII absorption features in the spectrum of Mrk 421 obtained with the Chandra Low Energy Transmission Grating Spectrometer (LETGS). We evaluate those claims in the context of a high quality spectrum of the same source obtained with the Reflection Grating Spectrometer (RGS) on XMM-Newton. The data comprise over 955~ksec of usable exposure time and more than 26000 counts per 50 milliAngstroms at 21.6 Angstroms. We concentrate on the spectrally clean region (21.3 < lambda < 22.5 Angstrom) where sharp features due to the astrophysically abundant O VII may reveal an intervening, warm-hot intergalactic medium (WHIM). In spite of the fact that the sensitivity of the RGS data is higher than that of the original LETGS data presented by Nicastro et al., we do not confirm detection of any of the intervening systems claimed to date. Rather, we detect only three unsurprising, astrophysically expected features down to the Log(N)~14.6 (3sigma) s...

  6. On the Putative Detection of Z>0 X-Ray Absorption Features in the Spectrum of Mrk 421

    Energy Technology Data Exchange (ETDEWEB)

    Rasmussen, Andrew P.; /SLAC /KIPAC, Menlo Park; Kahn, Steven M.; /SLAC /KIPAC, Menlo Park /Stanford U., Phys. Dept.; Paerels, Frits; /Columbia U., Astron. Astrophys.; Herder, Jan Willem den; Kaastra, Jelle; de Vries, Cor; /SRON, Utrecht

    2006-04-28

    In a series of papers, Nicastro et al. have claimed the detection of z > 0 O VII absorption features in the spectrum of Mrk 421 obtained with the Chandra Low Energy Transmission Grating Spectrometer (LETGS). We evaluate those claims in the context of a high quality spectrum of the same source obtained with the Reflection Grating Spectrometer (RGS) on XMM-Newton. The data comprise over 955 ksec of usable exposure time and more than 2.6 x 10{sup 4} counts per 50 m{angstrom} at 21.6 {angstrom}. We concentrate on the spectrally clean region (21.3 < {lambda} < 22.5 {angstrom}) where sharp features due to the astrophysically abundant O VII may reveal an intervening, warm-hot intergalactic medium (WHIM). In spite of the fact that the sensitivity of the RGS data is higher than that of the original LETGS data presented by Nicastro et al., we do not confirm detection of any of the intervening systems claimed to date. Rather, we detect only three unsurprising, astrophysically expected features down to the log (N{sub i}) {approx} 14.6 (3{sigma}) sensitivity level. Each of the two purported WHIM features is rejected with a statistical confidence that exceeds that reported for its initial detection. While we can not rule out the existence of fainter, WHIM related features in these spectra, we suggest that previous discovery claims were premature. A more recent paper by Williams et al. claims to have demonstrated that the RGS data we analyze here do not have the resolution or statistical quality required to confirm or deny the LETGS detections. We show that the Williams et al. reduction of the RGS data was highly flawed, leading to an artificial and spurious degradation of the instrument response. We carefully highlight the differences between our analysis presented here and those published by Williams et al.

  7. Gamma spectrometric assessment of nuclear fuel

    Science.gov (United States)

    Krištof, Edvard; Pregl, Gvido

    1990-12-01

    A description is given of a gamma spectrometric technique which has been developed with the aim of determining the amount of a certain radioactive fission product taking into consideration local variations of the linear attenuation coefficient of gamma rays. Also, an experiment using a fuel element of the TRIGA Mark II reactor in Ljubljana is presented.

  8. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    Energy Technology Data Exchange (ETDEWEB)

    Doyle, Adriana [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil); Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N. [Leopoldo Américo Miguez de Mello Research Center — Petrobras (CENPES), Cidade Universitária, Quadra 7, Ilha do Fundão, Rio de Janeiro 21949-900 (Brazil); Aucélio, Ricardo Q., E-mail: aucelior@puc-rio.br [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil)

    2013-08-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated.

  9. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    International Nuclear Information System (INIS)

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated

  10. Gamow-Teller decay and nuclear deformation: implementing of a new total absorption spectrometer, study of isotopes N {approx_equal} Z krypton and strontium; Decroissance Gamow-Teller et deformation nucleaire: mise en oeuvre d'un nouveau spectrometre a absorption totale, etude d'isotopes N {approx_equal} Z de krypton et strontium

    Energy Technology Data Exchange (ETDEWEB)

    Poirier, E

    2002-12-01

    Nuclei with A {approx} 70 along the N=Z line are known to be the scene of phenomena closely related to the nuclear deformation and are of particular interest since theoretical mean field calculations predict that a large part of the Gamow-Teller resonance might be located below the ground state of the mother nucleus and then be accessible through {beta}-decay studies. These results have shown the effect of the shape of the ground state on the intensity of the Gamow-Teller strength. Thus, the experimental determination, through {delta}-decay, of the Gamow-Teller strength distribution and the comparison to the theoretical predictions allow to pin down the quadrupolar deformation parameter of the ground state of the parent nucleus. In order to study the neutron deficient isotopes of krypton (A=72,73,74,75) and strontium (A=76,77,78) and to establish the {beta}-strength on the full energy range, a new total absorption spectrometer (TAgS) has been built in the frame of an international collaboration and installed at the (SOLDE/CERN mass separator. For the data analysis, the response function R of the spectrometer has been calculated by means of Monte-Carlo simulations, based on the GEANT4 code, and of a statistical description of the level scheme in the daughter nucleus. The {beta}-feeding distribution has been obtained from experimental spectra through a method based on Bayes theorem and then converted into Gamow-Teller strength. The results coming from the {sup 74}Kr decay analysis allow to describe the ground state of such a nucleus as the coexistence of an oblate shape and of a prolate shape. In the case of {sup 76}Sr, the experimental Gamow-Teller strength distribution strongly indicates a prolate deformation. (author)

  11. A novel microwave absorption and dielectric spectrum detection technology in photoelectron dynamic study for solar cells

    Institute of Scientific and Technical Information of China (English)

    LI Xiaowei; SUN Shuxu; LAI Weidong; ZHANG Rongxiang; DAI Xiuhong; JIANG Xiaoli

    2006-01-01

    The photoelectron property is directly related to the light-energy conversion efficiency of solar cells. In this paper, the photoelectron dynamic of semiconductor was analyzed. The diffusion of electrons has influence on the dielectric function of the solar cell material. And the amplitude variance of the imaginary andreal part of the dielectric function is in direct proportion to the dynamic process of free and shallow-trapped electrons. Based on the untouched detection technique, the method is present to detect the amplitude change of the microwave signal which is passing through the material whose dielectric function changes after exposure. A35GHz oscillator was used as a microwave source. The absorptionand dispersion microwave signals, which contain the dynamic information of free and shallow-trapped electron signal, are split respectively with phase-sensitive instrument. The photoelectron character of n-type Si(100) thin film was investigated by the novel equipment, and the lifetime of different kinds of electronswith the resolution of 1 ns was obtained. The equipment can be directly used inthe study of the optoelectronic conversion mechanism of solar cells.

  12. In-situ detection of tropospheric OH radicals by folded long-path laser absorption. Results from the POPCORN Field Campaign in August 1994

    Science.gov (United States)

    Dorn, H.-P.; Brandenburger, U.; Brauers, T.; Hausmann, M.; Ehhalt, D. H.

    Ground based in-situ measurements of tropospheric hydroxyl radicals were conducted by folded long-path laser absorption as part of the field campaign POPCORN in August 1994. The OH instrument used an open optical multiple-reflection cell of 38.5 m base length through which the laser beam was passed up to 80 times. The broadband emission of a short-pulse UV laser together with a multichannel detection system allowed the simultaneous observation of six OH absorption lines in a spectral interval of Δλ≃0.24 nm at 308.1nm (A²Σ+,υ‧ = 0← X²Π,υ″ = 0 transition). Along with the OH radicals, the trace gases SO2, HCHO, and naphthalene were measured by this technique. The large spectral detection range covered a multitude of rotational absorption lines of these trace gases which were all used for multicomponent analysis, thus allowing a specific and sensitive detection of tropospheric OH radicals. An average 2σ detection limit of 1.5 × 106 OH/cm³ for an integration time of 200 seconds and an absorption light path length of 1848 m was determined from the field measurements. In total, 392 OH data were obtained by long-path absorption during 16 days of field measurements. The observed OH concentrations reached peak values of 13 × 106 cm-3 at noon.

  13. Determination of Lead Content in Phosphate Rock and Concentrate Rock——Flame Atomic Absorption Spectrometric Method%火焰原子吸收光谱法测定磷矿石和精磷矿中的铅含量

    Institute of Scientific and Technical Information of China (English)

    沈治荣; 梁聪; 甘丽; 何红莲

    2011-01-01

    This article describes determination of trace harmful heavy metal-lead element in phosphate rock and concentrate rock with flame atomic absorption spectrometry method.The relative standard deviation of this method is 3.1~14.2%,recovery rate is 90%~104%,the sample detection limit is 0.0008%.The method is accurate,fast,easy,make up for method of determination lead in phosphate rock.It provides effective control method for production of feed additives and fertilizers and so on.%研究了用火焰原子吸收光谱法测定磷矿石或磷精矿中微量的铅的检测方法。此方法的相对标准偏差为3.1%-14.2%,回收率为90%-104%,样品检测下限为0.0008%。

  14. Identification of organic iodocompounds in the PUREX process with the help of methods for chromatographic separation and spectrometric detection as well as characterization of their behavior during extraction. Final report

    International Nuclear Information System (INIS)

    In the system HNO3 KI, Dodecan and TBP the radiolytic reactive behaviour of the described compounds during the dissolution of nuclear fuel elements was simulated. External γ-irradiation gave the best informations. As a consequence of radiolyticly induced reactions several volatile and non-volatile iodoorganic compounds like iodoalkanes, iodonitroalkanes and iodonitroalkylphosphates are formed. They were separated by gaschromatography (GC) and high performance liquid chromatography (HPLC). For HPLC a special photolytic/electrochemical detector with comparable sensitivity like the electroncapture detector in the GC-field was developed. With the help of the two described chromatographic techniques the different iodoorganic compounds could be separated singularily or in groups of isomers. The separation of all compounds demands two-dimensional chromatographies including the capillary-SFC, which was not available for this project. Most of the iodoorganic compounds could be identified by comparison of the retention times of well known compounds. In the other cases, the compounds were studied mass-spectrometrically. Unfortunately all available ionisation techniques (EI; CI; FAB) were too hard for the labile C-I-bond. Therefore an identification of these compounds was not possible. In any case, instructive fingerprint spectra are available enabling relationships between the generation of the iodoorganic compounds and the reaction conditions during their formation. (orig.)

  15. Improved limit of detection and quantitation development and validation procedure for quantification of zinc in Insulin by atomic absorption spectrometry.

    Science.gov (United States)

    Qadir, Muhammad Abdul; Ahmed, Mahmood; Haq, Iftikharul; Ahmed, Saghir

    2015-05-01

    A simple and expeditious analytical method for determination of zinc in human insulin isophane suspension by flame atomic absorption spectrophotometer (FAAS) was validated. The method was carried out on atomic absorption spectrometer with 0.4 nm bandwidth, 1.0 filter factor on deuterium (D2) background correction. The integration time was set at 3.0 second with 5.0 mA lamp current. The parameters of method validation showed adequate linearity, efficiency and relative standard deviation values were between 0.64%-1.69% (n=7), 1.31%-1.58% (n=10) for repeatability and intermediate precision respectively. The limit of detection 0.0032 μg/mL, 0.0173 μg/mL, 0.0231 μg/mL and limit of quantitation 0.0107μg/mL, 0.0578 μg/mL, 0.0694 μg/mL based on signal to noise (SN), calibration curve method (CCM) and fortification of blank (FB) were obtained respectively. The percentages of recovery for low, medium and high spiked concentration levels of zinc in human insulin were 99.38 ± 0.04 to 100.3 ± 0.03, 98.45 ± 0.38 to 100.3 ± 0.07 and 99.42 ± 0.03 to 99.42 ± 0.08 respectively. With the use of this method, five samples from each vial of human insulin isophane suspension were analyzed and the zinc content was determined. The zinc content were 22.1 ± 0.025 μg/mL and 24.3 ± 0.028 μg/mL which compliance the British Pharmacopoeia standard. PMID:26004720

  16. A Light-Emitting Diode- (LED-) Based Absorption Sensor for Simultaneous Detection of Carbon Monoxide and Carbon Dioxide.

    Science.gov (United States)

    Thurmond, Kyle; Loparo, Zachary; Partridge, William; Vasu, Subith S

    2016-06-01

    A sensor was developed for simultaneous measurements of carbon monoxide (CO) and carbon dioxide (CO2) fluctuations in internal combustion engine exhaust gases. This sensor utilizes low-cost and compact light-emitting diodes (LEDs) that emit in the 3-5 µm wavelength range. An affordable, fast response sensor that can measure these gases has a broad application that can lead to more efficient, fuel-flexible engines and regulation of harmful emissions. Light emission from LEDs is spectrally broader and more spatially divergent when compared to that of lasers, which presented many design challenges. Optical design studies addressed some of the non-ideal characteristics of the LED emissions. Measurements of CO and CO2 were conducted using their fundamental absorption bands centered at 4.7 µm and 4.3 µm, respectively, while a 3.6 µm reference LED was used to account for scattering losses (due to soot, window deposits, etc.) common to the three measurement LEDs. Instrument validation and calibration was performed using a laboratory flow cell and bottled-gas mixtures. The sensor was able to detect CO2 and CO concentration changes as small as 30 ppm and 400 ppm, respectively. Because of the many control and monitor species with infra-red absorption features, which can be measured using the strategy described, this work demonstrates proof of concept for a wider range of fast (250 Hz) and low-cost sensors for gas measurement and process monitoring. PMID:27091903

  17. Development and validation of highly selective screening and confirmatory methods for the qualitative forensic analysis of organic explosive compounds with high performance liquid chromatography coupled with (photodiode array and) LTQ ion trap/Orbitrap mass spectrometric detections (HPLC-(PDA)-LTQOrbitrap).

    Science.gov (United States)

    Xu, Xiaoma; Koeberg, Mattijs; Kuijpers, Chris-Jan; Kok, Eric

    2014-01-01

    An LTQ-Orbitrap FTMS is a new (hybrid) mass spectrometric (MS) analyzer. It allows for the acquisition of full scan MS(n) (n-stage fragmentations, n=1-n) spectra with the linear ion trap detector (LTQ) at high speed and/or with the Fourier Transform-detector (Orbitrap) with ultra high mass resolution (>60,000 at m/z17025 and NEN 7777). The methods are highly selective due to the simultaneous utilization of the Orbitrap FTMS and LTQ MS(2), both of which are highly selective detectors Tested explosive compounds can be detected in the molecular ion form by the Orbitrap analyzer with minimal mass interference in different matrices when using an extremely narrow mass tolerance detection window (≤2ppm). The identification of a detected compound follows an identification point system. Experimental results show that almost all explosive compounds meet the confirmation criteria (minimum 4 points) required for the positive identification by the DC 2002/657/EC. PMID:24438773

  18. Development and Application of a new Long Path Absorption Photometer (LOPAP) Instrument for the Sensitive Detection of NO2

    OpenAIRE

    Villena Tapia, Guillermo Harold

    2014-01-01

    A compact and simple instrument for the sensitive detection of NO2 in the atmosphere has been developed. NO2 is sampled in a stripping coil by a selective chemical reaction, converted into a highly absorbing dye, which is detected by long path absorption in a liquid core waveguide. Several interferences were quantified in the laboratory, which so far can all be neglected. The significant interferences against HONO and O3 were suppressed by using an upstream HONO/O3 -scrubber. ...

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

    Science.gov (United States)

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

    2016-05-01

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

  20. Bolometric detection of magnetoplasma resonances in microwave absorption by two-dimensional electron systems based on doping layer conductivity measurements in GaAs/AlGaAs heterostructures

    Energy Technology Data Exchange (ETDEWEB)

    Dorozhkin, S. I., E-mail: dorozh@issp.ac.ru; Sychev, D. V.; Kapustin, A. A. [Institute of Solid State Physics RAS, 142432 Chernogolovka, Moscow district (Russian Federation)

    2014-11-28

    We have implemented a new bolometric method to detect resonances in magneto-absorption of microwave radiation by two-dimensional electron systems (2DES) in selectively doped GaAs/AlGaAs heterostructures. Radiation is absorbed by the 2DES and the thermally activated conductivity of the doping layer supplying electrons to the 2DES serves as a thermometer. The resonant absorption brought about by excitation of the confined magnetoplasma modes appears as peaks in the magnetic field dependence of the low-frequency impedance measured between the Schottky gate and 2DES.

  1. Time-resolved detection of temperature, concentration, and pressure in a shock tube by intracavity absorption spectroscopy

    Science.gov (United States)

    Fjodorow, Peter; Fikri, Mustapha; Schulz, Christof; Hellmig, Ortwin; Baev, Valery M.

    2016-06-01

    In this paper, we demonstrate the first application of intracavity absorption spectroscopy (ICAS) for monitoring species concentration, total pressure, and temperature in shock-tube experiments. ICAS with a broadband Er3+-doped fiber laser is applied to time-resolved measurements of absorption spectra of shock-heated C2H2. The measurements are performed in a spectral range between 6512 and 6542 cm-1, including many absorption lines of C2H2, with a time resolution of 100 µs and an effective absorption path length of 15 m. Up to 18-times increase of the total pressure and a temperature rise of up to 1200 K have been monitored. Due to the ability of simultaneously recording many absorption lines in a broad spectral range, the presented technique can also be applied to multi-component analysis of transient single-shot processes in reactive gas mixtures in shock tubes, pulse detonation engines, or explosions.

  2. Evidence for ultra-fast outflows in radio-quiet AGNs: I - detection and statistical incidence of Fe K-shell absorption lines

    CERN Document Server

    Tombesi, F; Reeves, J N; Palumbo, G G C; Yaqoob, T; Braito, V; Dadina, M

    2010-01-01

    We performed a blind search for narrow absorption features at energies greater than 6.4 keV in a sample of 42 radio-quiet AGNs observed with XMM-Newton. We detect 36 narrow absorption lines on a total of 101 XMM-Newton EPIC pn observations. The number of absorption lines at rest-frame energies E>7 keV is 22. Their global probability to be generated by random fluctuations is very low, less than 3x10^-8, and their detection have been independently confirmed by a spectral analysis of the MOS data, with associated random probability <10^-7. We identify the lines as Fe XXV and Fe XXVI K-shell resonant absorption. They are systematically blue-shifted, with a velocity distribution ranging from zero up to 0.3c, with a peak and mean value at 0.1c. We detect variability of the lines on both EWs and blue-shifted velocities among different observations even on time-scales as short as a few days, possibly suggesting somewhat compact absorbers. Moreover, we find no significant correlation between the cosmological red-sh...

  3. Development and validation of highly selective screening and confirmatory methods for the qualitative forensic analysis of organic explosive compounds with high performance liquid chromatography coupled with (photodiode array and) LTQ ion trap/Orbitrap mass spectrometric detections (HPLC-(PDA)-LTQOrbitrap).

    Science.gov (United States)

    Xu, Xiaoma; Koeberg, Mattijs; Kuijpers, Chris-Jan; Kok, Eric

    2014-01-01

    An LTQ-Orbitrap FTMS is a new (hybrid) mass spectrometric (MS) analyzer. It allows for the acquisition of full scan MS(n) (n-stage fragmentations, n=1-n) spectra with the linear ion trap detector (LTQ) at high speed and/or with the Fourier Transform-detector (Orbitrap) with ultra high mass resolution (>60,000 at m/zphoto diode array (PDA) detection. Two methods for the forensic screening and confirmation of all common trace explosives in post-blast residues have been developed on this instrument using atmospheric pressure chemical ionization (APCI). In one run, the nitrogen-containing explosives are analyzed with the combination of "LC-(PDA)-APCI(-)-LTQ MS(2)/Orbitrap FTMS" (Method 1). In another run, peroxide explosives are analyzed with "LC-APCI(+)-LTQ MS(2)/Orbitrap FTMS" (Method 2). The performance of both methods has been validated according to procedures defined in the EU COMMISSION DECISION implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results (DC 2002/657/EC) and other standards (NEN 17025 and NEN 7777). The methods are highly selective due to the simultaneous utilization of the Orbitrap FTMS and LTQ MS(2), both of which are highly selective detectors Tested explosive compounds can be detected in the molecular ion form by the Orbitrap analyzer with minimal mass interference in different matrices when using an extremely narrow mass tolerance detection window (≤2ppm). The identification of a detected compound follows an identification point system. Experimental results show that almost all explosive compounds meet the confirmation criteria (minimum 4 points) required for the positive identification by the DC 2002/657/EC.

  4. Column solid phase extraction and flame atomic absorption spectrometric determination of manganese(II) and iron(III) ions in water, food and biological samples using 3-(1-methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid on synthesized graphene oxide.

    Science.gov (United States)

    Pourjavid, Mohammad Reza; Sehat, Ali Akbari; Arabieh, Masoud; Yousefi, Seyed Reza; Hosseini, Majid Haji; Rezaee, Mohammad

    2014-02-01

    A modified, selective, highly sensitive and accurate procedure for the determination of trace amounts of manganese and iron ions is established in the presented work. 3-(1-Methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid (MPPC) and graphene oxide (GO) were used in a glass column as chelating reagent and as adsorbent respectively prior to their determination by flame atomic absorption spectrometry. The adsorption mechanism of titled metals complexes on GO was investigated by using computational chemistry approach based on PM6 semi-empirical potential energy surface (PES). The effect of some parameters including pH, flow rate and volume of sample and type, volume and concentration of eluent, as well as the adsorption capacity of matrix ions on the recovery of Mn(II) and Fe(III) was investigated. The limit of detection was 145 and 162 ng L(-1) for Mn(II) and Fe(III), respectively. Calibration was linear over the range of 0.31-355 μg L(-1) for Mn(II) and 0.34-380 μg L(-1) for Fe(III) ions. The method was successfully applied for the determination of understudied ions in water, food and biological samples. PMID:24411390

  5. Column solid phase extraction and flame atomic absorption spectrometric determination of manganese(II) and iron(III) ions in water, food and biological samples using 3-(1-methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid on synthesized graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Pourjavid, Mohammad Reza, E-mail: pourjavid@gmail.com [NFCRS, Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of); Sehat, Ali Akbari [Department of Analytical Chemistry, Faculty of Chemistry, University College of Science, University of Tehran, P.O. Box 14155-6455, Tehran (Iran, Islamic Republic of); Arabieh, Masoud; Yousefi, Seyed Reza; Hosseini, Majid Haji; Rezaee, Mohammad [NFCRS, Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of)

    2014-02-01

    A modified, selective, highly sensitive and accurate procedure for the determination of trace amounts of manganese and iron ions is established in the presented work. 3-(1-Methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid (MPPC) and graphene oxide (GO) were used in a glass column as chelating reagent and as adsorbent respectively prior to their determination by flame atomic absorption spectrometry. The adsorption mechanism of titled metals complexes on GO was investigated by using computational chemistry approach based on PM6 semi-empirical potential energy surface (PES). The effect of some parameters including pH, flow rate and volume of sample and type, volume and concentration of eluent, as well as the adsorption capacity of matrix ions on the recovery of Mn(II) and Fe(III) was investigated. The limit of detection was 145 and 162 ng L{sup −1} for Mn(II) and Fe(III), respectively. Calibration was linear over the range of 0.31–355 μg L{sup −1} for Mn(II) and 0.34–380 μg L{sup −1} for Fe(III) ions. The method was successfully applied for the determination of understudied ions in water, food and biological samples. - Highlights: • We use synthesized graphene oxide as adsorbent for SPE of Mn(II) and Fe(III) ions. • Adsorption mechanism was investigated by PM6 semi-empirical potential energy surface. • Detection limits were 145 and 162 ng L{sup −1} for Mn and Fe, respectively. • The preconcentration factor was 325 and sample flow rate is 8 mL min{sup −1}. • It was successfully applied to the determination of Mn and Fe ions in real samples.

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

    DEFF Research Database (Denmark)

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

    2005-01-01

    . The samples are adjusted to pH 5.0 on-line in the system for optimum operation. The target ions are adsorbed by chelation on the surface of the beads, contained in a 20 mul microcolumn within the LOV, and following elution by 50 mul 2M nitric acid, the eluate is, as sandwiched by air segments, introduced...

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

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Jensen, Rikard;

    2006-01-01

    methodology showed 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....

  8. Gaia and its spectrometric challenge

    International Nuclear Information System (INIS)

    The Gaia program was kicked off at the beginning of 2006 and is now reaching a phase of construction and integration for a launch at the end of 2011, to reach the L2 point several months later. Apart from that industrial activity, the European astronomical community is actively preparing the data treatment and in particular how to extract the astrophysical parameter outputs from the use of the spectrographs on board the satellite. This work consists of the realization of algorithms to extract fundamental parameters of the detected source points with the help of an extensive grid of synthetic spectral libraries. The number of these estimated fundamental parameters and their accuracy depend on the ability of the algorithms to treat the spectra and to compare them with the computed ones, and also on the quality of the synthetic spectra themselves. Then, on the one hand a huge effort is underway to produce these extensive grids of one-dimensional (1D) local thermodynamic equilibrium (LTE) spectra of stars, galaxies, quasi-stellar objects and asteroids, and on the other hand, new physics is tested in the atmosphere model of stars to improve the theoretical libraries. An example of the questions we need to answer is: do we need 3D non-local thermodynamic equilibrium (NLTE) modelling? If yes, the libraries will then be improved by adding corrections checked on dedicated standard stars. Shall we be able to implement this new physics in a reasonable time? This is another challenge.

  9. Mass spectrometric determination of early and advanced glycation in biology.

    Science.gov (United States)

    Rabbani, Naila; Ashour, Amal; Thornalley, Paul J

    2016-08-01

    Protein glycation in biological systems occurs predominantly on lysine, arginine and N-terminal residues of proteins. Major quantitative glycation adducts are found at mean extents of modification of 1-5 mol percent of proteins. These are glucose-derived fructosamine on lysine and N-terminal residues of proteins, methylglyoxal-derived hydroimidazolone on arginine residues and N(ε)-carboxymethyl-lysine residues mainly formed by the oxidative degradation of fructosamine. Total glycation adducts of different types are quantified by stable isotopic dilution analysis liquid chromatography-tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring mode. Metabolism of glycated proteins is followed by LC-MS/MS of glycation free adducts as minor components of the amino acid metabolome. Glycated proteins and sites of modification within them - amino acid residues modified by the glycating agent moiety - are identified and quantified by label-free and stable isotope labelling with amino acids in cell culture (SILAC) high resolution mass spectrometry. Sites of glycation by glucose and methylglyoxal in selected proteins are listed. Key issues in applying proteomics techniques to analysis of glycated proteins are: (i) avoiding compromise of analysis by formation, loss and relocation of glycation adducts in pre-analytic processing; (ii) specificity of immunoaffinity enrichment procedures, (iii) maximizing protein sequence coverage in mass spectrometric analysis for detection of glycation sites, and (iv) development of bioinformatics tools for prediction of protein glycation sites. Protein glycation studies have important applications in biology, ageing and translational medicine - particularly on studies of obesity, diabetes, cardiovascular disease, renal failure, neurological disorders and cancer. Mass spectrometric analysis of glycated proteins has yet to find widespread use clinically. Future use in health screening, disease diagnosis and therapeutic monitoring, and

  10. New Perspective on Galaxy Outflows From the First Detection of Both Intrinsic and Traverse Metal-Line Absorption

    CERN Document Server

    Kacprzak, Glenn G; Bouché, Nicolas; Churchill, Christopher W; Cooke, Jeff; LeReun, Audrey; Schroetter, Ilane; Ho, Stephanie H; Klimek, Elizabeth

    2014-01-01

    We present the first observation of a galaxy (z=0.2) that exhibits metal-line absorption back-illuminated by the galaxy ("down-the-barrel") and transversely by a background quasar at a projected distance of 58 kpc. Both absorption systems, traced by MgII, are blueshifted relative to the galaxy systemic velocity. The quasar sight-line, which resides almost directly along the projected minor axis of the galaxy, probes MgI and MgII absorption obtained from Keck/LRIS and Lya, SiII and SiIII absorption obtained from HST/COS. For the first time, we combine two independent models used to quantify the outflow properties for down-the-barrel and transverse absorption. We find that the modeled down-the-barrel deprojected outflow velocities range between $V_{dtb}=45-255$ km/s. The transverse bi-conical outflow model, assuming constant-velocity flows perpendicular to the disk, requires wind velocities $V_{outflow}=40-80$ km/s to reproduce the transverse MgII absorption kinematics, which is consistent with the range of $V_...

  11. V oxidation state in Fe-Ti oxides by high-energy resolution fluorescence-detected X-ray absorption spectroscopy

    OpenAIRE

    Bordage, A.; Balan, Etienne; De Villiers, J.P.R.; Cromarty, R.; Juhin, A.; Carvallo, C.; Calas, G.; Raju, P. V. S.; Glatzel, P.

    2011-01-01

    The oxidation state of vanadium in natural and synthetic Fe-Ti oxides is determined using high-energy resolution fluorescence-detected X-ray absorption spectroscopy (HERFD-XAS). Eleven natural magnetite-bearing samples from a borehole of the Main Magnetite Layer of the Bushveld Complex (South Africa), five synthetic Fe oxide samples, and three natural hematite-bearing samples from Dharwar supergroup (India) are investigated. V K edge spectra were recorded on the ID26 beamline at the European ...

  12. Chandra view of the warm-hot intergalactic medium toward 1ES 1553+113: Absorption-line detections and identifications. I

    OpenAIRE

    F. Nicastro; Barcons, Xavier; Paerels, F. B. S.

    2013-01-01

    We present the first results from our pilot 500 ks Chandra Low Energy Transmission Grating Large Program observation of the soft X-ray brightest source in the z ≳ 0.4 sky, the blazar 1ES 1553+113, aimed to secure the first uncontroversial detections of the missing baryons in the X-rays. We identify a total of 11 possible absorption lines, with single-line statistical significances between 2.2σ and 4.1σ. Six of these lines are detected at high single-line statistical significance (3.6 ≤ σ ≤ 4....

  13. Chandra View of the Warm-Hot IGM toward 1ES 1553+113: Absorption Line Detections and Identifications (Paper I)

    CERN Document Server

    Nicastro, F; Krongold, Y; Mathur, S; Gupta, A; Danforth, C; Barcons, X; Borgani, S; Branchini, E; Cen, R; Davé, R; Kaastra, J; Paerels, F; Piro, L; Shull, J M; Takei, Y; Zappacosta, L

    2012-01-01

    About 30-40 percent of the expected number of baryons is still missing in the local Universe (z \\lesssim 0.4). They are predicted to be hiding in a web of intergalactic gas at temperatures of about 10^5-10^7 K (the WHIM). Detecting this matter has had limited success so far, because of its low-density and high temperature, which makes it difficult to detect with current far-ultraviolet and X-ray instrumentation. Here we present the first results from our pilot 500 ks Chandra-LETG observation of the soft X-ray brightest source in the z > 0.4 sky, the blazar 1ES 1553+113. We identify a total of 11 possible absorption lines, with single-line statistical significances between 2.2-4.1 sigma. Six of these lines are detected at high significance (3.6 < \\sigma < 4.1), while the remaining five are regarded as marginal detections in association with either other X-ray lines detected at higher significance and/or FUV signposts. Three of these lines are consistent with metal absorption at z~0. The remaining 8 lines...

  14. Evidence for ultra-fast outflows in radio-quiet AGNs. I. Detection and statistical incidence of Fe K-shell absorption lines

    Science.gov (United States)

    Tombesi, F.; Cappi, M.; Reeves, J. N.; Palumbo, G. G. C.; Yaqoob, T.; Braito, V.; Dadina, M.

    2010-10-01

    Context. Blue-shifted Fe K absorption lines have been detected in recent years between 7 and 10 keV in the X-ray spectra of several radio-quiet AGNs. The derived blue-shifted velocities of the lines can often reach mildly relativistic values, up to 0.2-0.4c. These findings are important because they suggest the presence of a previously unknown massive and highly ionized absorbing material outflowing from their nuclei, possibly connected with accretion disk winds/outflows. Aims: The scope of the present work is to statistically quantify the parameters and incidence of the blue-shifted Fe K absorption lines through a uniform analysis on a large sample of radio-quiet AGNs. This allows us to assess their global detection significance and to overcome any possible publication bias. Methods: We performed a blind search for narrow absorption features at energies greater than 6.4 keV in a sample of 42 radio-quiet AGNs observed with XMM-Newton. A simple uniform model composed by an absorbed power-law plus Gaussian emission and absorption lines provided a good fit for all the data sets. We derived the absorption lines parameters and calculated their detailed detection significance making use of the classical F-test and extensive Monte Carlo simulations. Results: We detect 36 narrow absorption lines on a total of 101 XMM-Newton EPIC pn observations. The number of absorption lines at rest-frame energies higher than 7 keV is 22. Their global probability to be generated by random fluctuations is very low, less than 3 × 10-8, and their detection have been independently confirmed by a spectral analysis of the MOS data, with associated random probability UFOs) those highly ionized absorbers with outflow velocities higher than 104 km s-1, then the majority of the lines are consistent with being associated to UFOs and the fraction of objects with detected UFOs in the whole sample is at least ~35%. This fraction is similar for type 1 and type 2 sources. The global covering fraction of

  15. Comparison of Tunable Diode Laser Absorption Spectroscopy and Isothermal Micro-calorimetry for Non-invasive Detection of Microbial Growth in Media Fills

    Science.gov (United States)

    Brueckner, David; Roesti, David; Zuber, Ulrich Georg; Schmidt, Rainer; Kraehenbuehl, Stefan; Bonkat, Gernot; Braissant, Olivier

    2016-01-01

    Two methods were investigated for non-invasive microbial growth-detection in intact glass vials as possible techniques for automated inspection of media-filled units. Tunable diode laser absorption spectroscopy (TDLAS) was used to determine microbially induced changes in O2 and CO2 concentrations within the vial headspaces. Isothermal microcalorimetry (IMC) allowed the detection of metabolic heat production. Bacillus subtilis and Streptococcus salivarius were chosen as test organisms. Parameters as robustness, sensitivity, comparability and time to detection (TtD) were evaluated to assess method adequacy. Both methods robustly detected growth of the tested microorganisms within less than 76 hours using an initial inoculum of automating the media-fill inspection, as larger throughput can be achieved. For routine use either TDLA or a combination of TDLA and TDLA should be considered. IMC may be helpful for replacing the sterility assessment of commercial drug products before release. PMID:27282661

  16. Probing Cu(I) in homogeneous catalysis using high-energy-resolution fluorescence-detected X-ray absorption spectroscopy.

    Science.gov (United States)

    Walroth, Richard C; Uebler, Jacob W H; Lancaster, Kyle M

    2015-06-18

    Metal-to-ligand charge transfer excitations in Cu(I) X-ray absorption spectra are introduced as spectroscopic handles for the characterization of species in homogeneous catalytic reaction mixtures. Analysis is supported by correlation of a spectral library to calculations and to complementary spectroscopic parameters.

  17. Microwave Digestion and Continuum Source Atomic Absorption Spectrometric Determination of Six Metal Elements in Medlar(Mespilus germanica L.) Fruit%微波消解-连续光源原子吸收法快速顺序测定枸杞果中的6种金属元素

    Institute of Scientific and Technical Information of China (English)

    高向阳; 王银娟; 卢彬

    2011-01-01

    A new rapid method was established to determine metal elements in medlar fruit by microwave digestion and continuum source atomic absorption spectrometry.Samples were subjected to microwave digestion before simultaneous determination of six metal elements,including iron,zinc,copper,manganese,cadmium and lead.The established method presented a limit of detection ranging from 0.006070 to 0.04975 μg/L.The precision RSDs were between 1.5% and 5.0%(n = 12).The mean spike recoveries for the six metal elements ranged from 86.68% to 111.7%(n = 6).This method has been used to simultaneously determine iron,zinc,copper,manganese,cadmium and lead in medlar fruit with the benefits of rapidity,simplicity and low cost and satisfying results.%建立一种微波消解-连续光源原子吸收法快速测定枸杞果中金属元素的新方法。通过微波消解快速处理样品,用连续光源原子吸收法同时顺序测定枸杞果中的铁、锌、铜、锰、镉、铅6种金属元素,并对仪器使用条件、金属元素含量、精密度、检出限、回收率等进行研究。结果表明:方法检出限为0.006 07 0~0.04975μg/L,RSD为1.5%~5.0%,回收率为86.68%~111.7%。该法用于枸杞中6种金属元素的同时顺序测定,具有快速、简便、成本低廉等特点,分析结果令人满意。

  18. NEW PERSPECTIVE ON GALAXY OUTFLOWS FROM THE FIRST DETECTION OF BOTH INTRINSIC AND TRAVERSE METAL-LINE ABSORPTION

    Energy Technology Data Exchange (ETDEWEB)

    Kacprzak, Glenn G.; Cooke, Jeff [Swinburne University of Technology, Victoria 3122 (Australia); Martin, Crystal L.; Ho, Stephanie H. [Physics Department, University of California, Santa Barbara, CA 93106 (United States); Bouché, Nicolas; LeReun, Audrey; Schroetter, Ilane [CNRS, Institut de Recherche en Astrophysique et Planétologie (IRAP) de Toulouse, 14 Avenue E. Belin, F-31400 Toulouse (France); Churchill, Christopher W.; Klimek, Elizabeth, E-mail: gkacprzak@astro.swin.edu.au [New Mexico State University, Las Cruces, NM 88003 (United States)

    2014-09-01

    We present the first observation of a galaxy (z = 0.2) that exhibits metal-line absorption back-illuminated by the galaxy (down-the-barrel) and transversely by a background quasar at a projected distance of 58 kpc. Both absorption systems, traced by Mg II, are blueshifted relative to the galaxy systemic velocity. The quasar sight line, which resides almost directly along the projected minor axis of the galaxy, probes Mg I and Mg II absorption obtained from the Keck/Low Resolution Imaging Spectrometer as well as Lyα, Si II, and Si III absorption obtained from the Hubble Space Telescope/Cosmic Origins Spectrograph. For the first time, we combine two independent models used to quantify the outflow properties for down-the-barrel and transverse absorption. We find that the modeled down-the-barrel deprojected outflow velocities range between V {sub dtb} = 45-255 km s{sup –1}. The transverse bi-conical outflow model, assuming constant-velocity flows perpendicular to the disk, requires wind velocities V {sub outflow} = 40-80 km s{sup –1} to reproduce the transverse Mg II absorption kinematics, which is consistent with the range of V {sub dtb}. The galaxy has a metallicity, derived from Hα and N II, of [O/H] = –0.21 ± 0.08, whereas the transverse absorption has [X/H] = –1.12 ± 0.02. The galaxy star formation rate is constrained between 4.6-15 M {sub ☉} yr{sup –1} while the estimated outflow rate ranges between 1.6-4.2 M {sub ☉} yr{sup –1} and yields a wind loading factor ranging between 0.1-0.9. The galaxy and gas metallicities, the galaxy-quasar sight-line geometry, and the down-the-barrel and transverse modeled outflow velocities collectively suggest that the transverse gas originates from ongoing outflowing material from the galaxy. The ∼1 dex decrease in metallicity from the base of the outflow to the outer halo suggests metal dilution of the gas by the time it reached 58 kpc.

  19. Femtosecond time-resolved X-ray absorption spectroscopy of liquid using a hard X-ray free electron laser in a dual-beam dispersive detection method.

    Science.gov (United States)

    Obara, Yuki; Katayama, Tetsuo; Ogi, Yoshihiro; Suzuki, Takayuki; Kurahashi, Naoya; Karashima, Shutaro; Chiba, Yuhei; Isokawa, Yusuke; Togashi, Tadashi; Inubushi, Yuichi; Yabashi, Makina; Suzuki, Toshinori; Misawa, Kazuhiko

    2014-01-13

    We present femtosecond time-resolved X-ray absorption spectroscopy of aqueous solution using a hard x-ray free electron laser (SACLA) and a synchronized Ti:sapphire laser. The instrumental response time is 200 fs, and the repetition rate of measurement is 10 Hz. A cylindrical liquid beam 100 μm in diameter of aqueous ammonium iron(III) oxalate solution is photoexcited at 400 nm, and the transient X-ray absorption spectra are measured in the K-edge region of iron, 7.10 - 7.26 keV, using a dual X-ray beam dispersive detection method. Each of the dual beams has the pulse energy of 1.4 μJ, and pump-induced absorbance change on the order of 10(-3) is successfully detected. The photoexcited iron complex exhibits a red shifted iron K-edge with the appearance time constant of 260 fs. The X-ray absorption difference spectra, with and without the pump pulses, are independent of time delay after 1.5 ps up to 100 ps, indicating that the photoexcited species is long-lived.

  20. 载人航天器密封舱微量有害气体质谱检测方法%Mass spectrometric detection of harmful trace gases in manned spacecraft capsule

    Institute of Scientific and Technical Information of China (English)

    陈联; 邱家稳; 王丽红; 张晓曦

    2011-01-01

    Detection of multi -component harmful trace gases in manned spacecraft capsule by miniature vacuum mass spectrometer was introduced. Online monitoring of a variety of harmful trace gases in the capsule was realized through detecting the gas concentration. Experimental data of relative sensitivity of some gases such as toluene, dimethylbenzene, dichloromethane, methane and acetone were given and the experiment also verified that the minimum detectable concentration of before -mentioned gases can reach lppm. The results indicated that monitoring of harmful trace gas concentration by miniature vacuum mass spectrometer in manned spacecraft capsule is feasible.%介绍了采用小型真空质谱计进行载人航天器密封舱内多组分微量有害气体的检测方法.通过测量微量气体浓度,实现密封舱内多种微量有害气体在线监测.给出了甲苯、二甲苯、二氯甲烷、甲烷、丙酮等5种气体的相对灵敏度试验数据,验证了现有小型真空质谱计最小可检浓度可以达到1ppm要求.研究结果表明,采用小型真空质谱计进行舱内微量有害气体浓度监测是可行的.

  1. CHANDRA VIEW OF THE WARM-HOT INTERGALACTIC MEDIUM TOWARD 1ES 1553+113: ABSORPTION-LINE DETECTIONS AND IDENTIFICATIONS. I

    Energy Technology Data Exchange (ETDEWEB)

    Nicastro, F.; Zappacosta, L. [Osservatorio Astronomico di Roma-INAF, Via di Frascati 33, I-00040 Monte Porzio Catone, RM (Italy); Elvis, M. [Harvard-Smithsonian Center for Astrophysics, 60 Garden St., MS-04, Cambridge, MA 02138 (United States); Krongold, Y. [Instituto de Astronomia, Universidad Nacional Autonoma de Mexico, Mexico City Mexico (Mexico); Mathur, S.; Gupta, A. [Ohio State University, Columbus, OH (United States); Danforth, C.; Shull, J. M. [CASA, Department of Astrophysical and Planetary Sciences, University of Colorado, 389-UCB, Boulder, CO 80309 (United States); Barcons, X. [Instituto de Fisica de Cantabria (CSIC-UC), E-39005 Santander (Spain); Borgani, S. [Dipartimento di Astronomia dell' Universita di Trieste, Via G.B. Tiepolo 11, I-34131 Trieste (Italy); Branchini, E. [Dipartimento di Fisica ' ' E. Amaldi' ' , Universita degli Studi ' ' Roma Tre' ' , via della Vasca Navale 84, I-00146 Roma (Italy); Cen, R. [Princeton University Observatory, Princeton, NJ 08544 (United States); Dave, R. [Astronomy Department, University of Arizona, Tucson, AZ 85721 (United States); Kaastra, J. [SRON Netherlands Institute for Space Research, Sorbonnelaan 2, 3584 CA, Utrecht (Netherlands); Paerels, F. [Columbia Astrophysics Laboratory and Department of Astronomy, Columbia University, 550 West 120th Street, New York, NY 10027 (United States); Piro, L. [INAF-IAPS, Via del Fosso del Cavaliere 100, I-00133 Roma (Italy); Takei, Y. [Institute of Space and Astronautical Science, Japan Aerospace Exploration Agency, 3-1-1 Yoshinodai, Chuo-ku, Sagamihara, Kanagawa 252-5210 (Japan)

    2013-06-01

    We present the first results from our pilot 500 ks Chandra Low Energy Transmission Grating Large Program observation of the soft X-ray brightest source in the z {approx}> 0.4 sky, the blazar 1ES 1553+113, aimed to secure the first uncontroversial detections of the missing baryons in the X-rays. We identify a total of 11 possible absorption lines, with single-line statistical significances between 2.2{sigma} and 4.1{sigma}. Six of these lines are detected at high single-line statistical significance (3.6 {<=} {sigma} {<=} 4.1), while the remaining five are regarded as marginal detections in association with either other X-ray lines detected at higher significance and/or far-ultraviolet (FUV) signposts. Three of these lines are consistent with metal absorption at z {approx_equal} 0, and we identify them with Galactic O I and C II. The remaining eight lines may be imprinted by intervening absorbers and are all consistent with being high-ionization counterparts of FUV H I and/or O VI intergalactic medium signposts. In particular, five of these eight possible intervening absorption lines (single-line statistical significances of 4.1{sigma}, 4.1{sigma}, 3.9{sigma}, 3.8{sigma}, and 2.7{sigma}), are identified as C V and C VI K{alpha} absorbers belonging to three WHIM systems at z{sub X} = 0.312, z{sub X} = 0.237, and (z{sub X} ) = 0.133, which also produce broad H I (and O VI for the z{sub X} = 0.312 system) absorption in the FUV. For two of these systems (z{sub X} = 0.312 and 0.237), the Chandra X-ray data led the a posteriori discovery of physically consistent broad H I associations in the FUV (for the third system the opposite applies), so confirming the power of the X-ray-FUV synergy for WHIM studies. The true statistical significances of these three X-ray absorption systems, after properly accounting for the number of redshift trials, are 5.8{sigma} (z{sub X} = 0.312; 6.3{sigma} if the low-significance O V and C V K{beta} associations are considered), 3.9{sigma} (z

  2. Intensity-Stabilized Fast-Scanned Direct Absorption Spectroscopy Instrumentation Based on a Distributed Feedback Laser with Detection Sensitivity down to 4 × 10−6

    Science.gov (United States)

    Zhao, Gang; Tan, Wei; Jia, Mengyuan; Hou, Jiajuan; Ma, Weiguang; Dong, Lei; Zhang, Lei; Feng, Xiaoxia; Wu, Xuechun; Yin, Wangbao; Xiao, Liantuan; Axner, Ove; Jia, Suotang

    2016-01-01

    A novel, intensity-stabilized, fast-scanned, direct absorption spectroscopy (IS-FS-DAS) instrumentation, based on a distributed feedback (DFB) diode laser, is developed. A fiber-coupled polarization rotator and a fiber-coupled polarizer are used to stabilize the intensity of the laser, which significantly reduces its relative intensity noise (RIN). The influence of white noise is reduced by fast scanning over the spectral feature (at 1 kHz), followed by averaging. By combining these two noise-reducing techniques, it is demonstrated that direct absorption spectroscopy (DAS) can be swiftly performed down to a limit of detection (LOD) (1σ) of 4 × 10−6, which opens up a number of new applications. PMID:27657082

  3. Intensity-Stabilized Fast-Scanned Direct Absorption Spectroscopy Instrumentation Based on a Distributed Feedback Laser with Detection Sensitivity down to 4 × 10−6

    Directory of Open Access Journals (Sweden)

    Gang Zhao

    2016-09-01

    Full Text Available A novel, intensity-stabilized, fast-scanned, direct absorption spectroscopy (IS-FS-DAS instrumentation, based on a distributed feedback (DFB diode laser, is developed. A fiber-coupled polarization rotator and a fiber-coupled polarizer are used to stabilize the intensity of the laser, which significantly reduces its relative intensity noise (RIN. The influence of white noise is reduced by fast scanning over the spectral feature (at 1 kHz, followed by averaging. By combining these two noise-reducing techniques, it is demonstrated that direct absorption spectroscopy (DAS can be swiftly performed down to a limit of detection (LOD (1σ of 4 × 10−6, which opens up a number of new applications.

  4. Liquid chromatography-mass spectrometric and liquid chromatography-tandem mass spectrometric determination of hallucinogenic indoles psilocin and psilocybin in "magic mushroom" samples.

    Science.gov (United States)

    Kamata, Tooru; Nishikawa, Mayumi; Katagi, Munehiro; Tsuchihashi, Hitoshi

    2005-03-01

    Accurate and sensitive analytical methods for psilocin (PC) and psilocybin (PB), tryptamine-type hallucinogens contained in "magic mushrooms," were investigated using liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS). The chromatographic separation on an ODS column and mass spectral information gave complete discrimination between PC and PB without derivatization. The mass spectrometric detection had a high sensitivity, and the tandem mass spectrometric detection provided more specificity and accuracy, as well as high sensitivity. The detection limits ranged from 1 to 25 pg by LC-MS in the selected ion monitoring mode, and the intra- and inter-day coefficients of variation were estimated to be 4.21-5.93% by LC-MS-MS in the selected reaction monitoring mode. By applying the present LC-MS-MS technique to four real samples, the contents of PC and PB were found to vary over a wide range (0.60-1.4 and 0.18-3.8 mg/g dry wt. for PC and PB, respectively) between samples.

  5. Detection of Highly Ionized Metal Absorption Lines in the Ultracompact X-ray Dipper 4U 1916-05

    CERN Document Server

    Juett, A M; Juett, Adrienne M.; Chakrabarty, Deepto

    2006-01-01

    We present the high-resolution Chandra X-ray Observatory persistent (non-dip) spectrum of 4U 1916-05 which revealed narrow absorption lines from hydrogenic neon, magnesium, silicon, and sulfur, in addition to the previous identified hydrogenic and helium-like iron absorption lines. This makes 4U 1916-05 only the second of the classical X-ray dipper systems to show narrow absorption lines from elements other than iron. We propose two possible explanations for the small measured line widths (>~ 500-2000 km s^{-1}), compared to the expected Keplerian velocities (> 1000 km s^{-1}) of the accretion disk in this 50-min orbital period system, and lack of wavelength shifts (>~ 250 km s^{-1}). First, the ionized absorber may be stationary. Alternatively, the line properties may measure the relative size of the emission region. From this hypothesis, we find that the emission region is constrained to be >~ 0.25 times the radial extent of the absorber. Our results also imply that the ionized absorber spans a range of ion...

  6. K-H_2 Quasi-molecular absorption detected in the T-dwarf epsilon Indi Ba

    CERN Document Server

    Allard, France; Homeier, Derek; Kielkopf, John; McCaughrean, Mark J; Spiegelman, Fernand

    2007-01-01

    T-type dwarfs present a broad and shallow absorption feature centred around 6950 A in the blue wing of the K doublet at 0.77 micron which resembles in depth and shape the satellite absorption predicted by detailed collisional broadening profiles. In our previous work, the predicted line satellite position was however somewhat too blue compared to the observed feature. In this paper we investigate whether new calculations of the energy surfaces of the potentials in the K-H_2 system, including spin-orbit coupling, result in a closer coincidence of the satellite with the observed position. We also investigate the extent to which CaH absorption bands contribute to the feature. We present model atmospheres and synthetic spectra, including gravitational settling for an improved description of depth-dependent abundances of refractory elements, and based on new K-H_2 line profiles using improved interaction potentials. By comparison with a high signal-to-noise optical spectrum of the T1 dwarf epsilon Indi Ba, we find...

  7. Chandra View of the Warm-hot Intergalactic Medium toward 1ES 1553+113: Absorption-line Detections and Identifications. I.

    Science.gov (United States)

    Nicastro, F.; Elvis, M.; Krongold, Y.; Mathur, S.; Gupta, A.; Danforth, C.; Barcons, X.; Borgani, S.; Branchini, E.; Cen, R.; Davé, R.; Kaastra, J.; Paerels, F.; Piro, L.; Shull, J. M.; Takei, Y.; Zappacosta, L.

    2013-06-01

    We present the first results from our pilot 500 ks Chandra Low Energy Transmission Grating Large Program observation of the soft X-ray brightest source in the z >~ 0.4 sky, the blazar 1ES 1553+113, aimed to secure the first uncontroversial detections of the missing baryons in the X-rays. We identify a total of 11 possible absorption lines, with single-line statistical significances between 2.2σ and 4.1σ. Six of these lines are detected at high single-line statistical significance (3.6 X-ray lines detected at higher significance and/or far-ultraviolet (FUV) signposts. Three of these lines are consistent with metal absorption at z ~= 0, and we identify them with Galactic O I and C II. The remaining eight lines may be imprinted by intervening absorbers and are all consistent with being high-ionization counterparts of FUV H I and/or O VI intergalactic medium signposts. In particular, five of these eight possible intervening absorption lines (single-line statistical significances of 4.1σ, 4.1σ, 3.9σ, 3.8σ, and 2.7σ), are identified as C V and C VI Kα absorbers belonging to three WHIM systems at zX = 0.312, zX = 0.237, and langzX rang = 0.133, which also produce broad H I (and O VI for the zX = 0.312 system) absorption in the FUV. For two of these systems (zX = 0.312 and 0.237), the Chandra X-ray data led the a posteriori discovery of physically consistent broad H I associations in the FUV (for the third system the opposite applies), so confirming the power of the X-ray-FUV synergy for WHIM studies. The true statistical significances of these three X-ray absorption systems, after properly accounting for the number of redshift trials, are 5.8σ (zX = 0.312; 6.3σ if the low-significance O V and C V Kβ associations are considered), 3.9σ (zX = 0.237), and 3.8σ (langzX rang = 0.133), respectively.

  8. Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

    International Nuclear Information System (INIS)

    Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 μg l-1 As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 μg l-1. Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l-1 acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l-1 HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 μg l-1 for As(III) and 0.3 μg l-1 for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 μg l-1 (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non-chromatographic and chromatographic procedures and the As

  9. Solid Phase Extraction of Lead Using Eggshell Membrane in Water Samples Prior to Graphite Furnace Atomic Absorption Spectrometric Determination%鸡蛋膜固相萃取-石墨炉原子吸收光谱法测定水样中的微量铅

    Institute of Scientific and Technical Information of China (English)

    刘金; 彭元; 陈红梅; 程先忠

    2012-01-01

    鸡蛋膜是由蛋白质组成的一种纤维状的生物膜.本研究利用扫描电镜和红外光谱对鸡蛋膜的结构进行分析表征,证实其具有网状结构,表面存在着—OH、—COOH、—NH2等官能团,能与一些金属离子产生吸附和交换作用.在pH =6的条件下,用蛋膜作吸附剂分离富集水样中的微量铅,5 mL 3%的硝酸进行洗脱,然后采用石墨炉原子吸收光谱法进行测定.实验中对吸附分离介质、溶液流速、蛋膜用量、洗脱剂浓度及共存离子的影响等条件进行了优化和讨论.在最佳的实验条件下,蛋膜对铅的富集倍数为30,方法检出限(3σ)为0.017 ng/mL,相对标准偏差(RSD,n=11)为3.45%,加标回收率为96.0% ~ 104.2%.与现行的分离富集方法相比,建立的方法具有简单、无毒、成本低的优点,用于实际水样中铅的分析能够获得满意的结果.%A chicken eggshell membrane (ESM) is composed of many protein fibers, and available in large quantities as a by-product of the food industry. According to a study by Scanning Electron Microscope ( SEM ) and Fourier Transform Infrared ( FTIR) Spectrometry, the ESM with an intricate lattice network of stable and water-insoluble fibers, and special functional groups such as hydroxyl ( —OH) , carboxyl ( —COOH) , aminol ( —NH2 ) , showed an excellent potential for adsorption and exchange of metal ions. In this paper, the ESM was applied to separate and enrich Pb (II) from a water sample under a pH of 6. The trace lead eluted by 5 mL 3% HN03 was determined by using Graphite Furnace Atomic Absorption Spectrometry ( GFAAS ) . Important parameters, such as the sample pH, sample flow rate, concentration and volume of eluent, and interference of coexisting ions were comprehensively studied and optimized. Under the optimized conditions, an enrichment factor of 30 was obtained. The method detection limit for lead was 0.017 ng/mL (3

  10. Detection of water absorption in the dayside atmosphere of HD 189733 b using ground-based high-resolution spectroscopy at 3.2 microns

    CERN Document Server

    Birkby, J L; Brogi, M; de Mooij, E J W; Schwarz, H; Albrecht, S; Snellen, I A G

    2013-01-01

    We report a 5 sigma detection of water absorption features in the dayside spectrum of the hot Jupiter HD 189733 b. We used high-resolution (R~100,000) spectra taken at 3.2 microns with CRIRES on the VLT to trace the radial velocity shift of the water features in the planet's dayside atmosphere during 5 hours of its 2.2 day orbit as it approached secondary eclipse. Despite considerable telluric contamination in this wavelength regime, we detect the signal within our uncertainties at the expected combination of systemic velocity (Vsys=-3 +5-6 km/s) and planet orbital velocity (Kp=154 +14-10 km/s), and determine a H2O line contrast ratio of (1.3+/-0.2)x10^-3 with respect to the stellar continuum. We find no evidence of significant absorption or emission from other carbon-bearing molecules, such as methane, although we do note a marginal increase in the significance of our detection with the inclusion of carbon dioxide in our template spectrum. This result demonstrates that ground-based, high-resolution spectrosc...

  11. Short-lived species detection of nitrous acid by external-cavity quantum cascade laser based quartz-enhanced photoacoustic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Yi, Hongming [Laboratoire de Physicochimie de l' Atmosphère, Université du Littoral Côte d' Opale, 189A, Av. Maurice Schumann, 59140 Dunkerque (France); Laboratory of Atmospheric Physico-Chemistry, Anhui Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, P.O. Box 1125, 350 Shushanhu Road, Hefei, Anhui 230031 (China); Maamary, Rabih; Fertein, Eric; Chen, Weidong, E-mail: chen@univ-littoral.fr [Laboratoire de Physicochimie de l' Atmosphère, Université du Littoral Côte d' Opale, 189A, Av. Maurice Schumann, 59140 Dunkerque (France); Gao, Xiaoming [Laboratory of Atmospheric Physico-Chemistry, Anhui Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, P.O. Box 1125, 350 Shushanhu Road, Hefei, Anhui 230031 (China); Sigrist, Markus W. [ETH Zurich, Institute for Quantum Electronics, HPT H4.1, Auguste-Piccard-Hof 1, CH-8093 Zürich (Switzerland)

    2015-03-09

    Spectroscopic detection of short-lived gaseous nitrous acid (HONO) at 1254.85 cm{sup −1} was realized by off-beam coupled quartz-enhanced photoacoustic spectroscopy (QEPAS) in conjunction with an external cavity quantum cascade lasers (EC-QCL). High sensitivity monitoring of HONO was performed within a very small gas-sample volume (of ∼40 mm{sup 3}) allowing a significant reduction (of about 4 orders of magnitude) of air sampling residence time which is highly desired for accurate quantification of chemically reactive short-lived species. Calibration of the developed QEPAS-based HONO sensor was carried out by means of lab-generated HONO samples whose concentrations were determined by direct absorption spectroscopy involving a ∼109.5 m multipass cell and a distributed feedback QCL. A minimum detection limit (MDL) of 66 ppbv (1 σ) HONO was achieved at 70 mbar using a laser output power of 50 mW and 1 s integration time, which corresponded to a normalized noise equivalent absorption coefficient of 3.6 × 10{sup −8 }cm{sup −1} W/Hz{sup 1/2}. This MDL was down to 7 ppbv at the optimal integration time of 150 s. The corresponding 1σ minimum detected absorption coefficient is ∼1.1 × 10{sup −7 }cm{sup −1} (MDL ∼ 3 ppbv) in 1 s and ∼1.1 × 10{sup −8 }cm{sup −1} (MDL ∼ 330 pptv) in 150 s, respectively, with 1 W laser power.

  12. Simultaneous derivatization and extraction of chlorophenols in water samples with up-and-down shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography/mass spectrometric detection.

    Science.gov (United States)

    Wang, Ke-Deng; Chen, Pai-Shan; Huang, Shang-Da

    2014-03-01

    A new up-and-down shaker-assisted dispersive liquid-liquid microextraction (UDSA-DLLME) for extraction and derivatization of five chlorophenols (4-chlorophenol, 4-chloro-2-methylphenol, 2,4-dichlorophenol, 2,4,6-trichloro-phenol, and pentachlorophenol) has been developed. The method requires minimal solvent usage. The relatively polar, water-soluble, and low-toxicity solvent 1-heptanol (12 μL) was selected as the extraction solvent and acetic anhydride (50 μL) as the derivatization reagent. With the use of an up-and-down shaker, the emulsification of aqueous samples was formed homogeneously and quickly. The derivatization and extraction of chlorophenols were completed simultaneously in 1 min. The common requirement of disperser solvent in DLLME could be avoided. After optimization, the linear range covered over two orders of magnitude, and the coefficient of determination (r (2)) was greater than 0.9981. The detection limit was from 0.05 to 0.2 μg L(-1), and the relative standard deviation was from 4.6 to 10.8 %. Real samples of river water and lake water had relative recoveries from 90.3 to 117.3 %. Other emulsification methods such as vortex-assisted, ultrasound-assisted, and manual shaking-enhanced ultrasound-assisted methods were also compared with the proposed UDSA-DLLME. The results revealed that UDSA-DLLME performed with higher extraction efficiency and precision compared with the other methods. PMID:23727731

  13. Determination of butyl- and phenyltin compounds in human urine by HS-SPME after derivatization with tetraethylborate and subsequent determination by capillary GC with microwave-induced plasma atomic emission and mass spectrometric detection.

    Science.gov (United States)

    Zachariadis, G A; Rosenberg, E

    2009-04-30

    A headspace solid-phase micro-extraction (HS-SPME) method was developed and optimized for gas chromatographic separation and determination of commonly found organotin compounds in human urine after potential exposure. Butyl- and phenyltin compounds were in situ derivatized to ethylated derivatives by sodium tetraethylborate (NaBEt(4)) directly in the urine matrix. The relevant parameters affecting the yield of the SPME procedure were examined using tetrabutyltin as internal standard. The method was optimized for direct use in the analysis of undiluted human urine samples and mono-, di- and tri-substituted butyl- and phenyltin compounds could be determined after a 15-min headspace extraction time at room temperature. The selectivity of the microwave-induced plasma atomic emission detector (MIP-AED) as an element specific detector in combination with the relatively selective sample preparation technique of HS-SPME allowed the interference-free detection of the organotin compounds in all cases. A quadrupole mass spectrometer was used in parallel experiments as a detector for the confirmation of the identity molecular structure of the eluted compounds. The performance characteristics of the developed method are given for the determination of mixtures of these compounds. Finally the proposed method was applied to the analysis of several human urine samples. PMID:19203626

  14. High-throughput sequential injection method for simultaneous determination of plutonium and neptunium in environmental solids using macroporous anion-exchange chromatography, followed by inductively coupled plasma mass spectrometric detection.

    Science.gov (United States)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per; Miró, Manuel

    2011-01-01

    This paper reports an automated analytical method for rapid and simultaneous determination of plutonium and neptunium in soil, sediment, and seaweed, with detection via inductively coupled plasma mass spectrometry (ICP-MS). A chromatographic column packed with a macroporous anion exchanger (AG MP-1 M) was incorporated in a sequential injection (SI) system for the efficient retrieval of plutonium, along with neptunium, from matrix elements and potential interfering nuclides. The sorption and elution behavior of plutonium and neptunium onto AG MP-1 M resin was compared with a commonly utilized AG 1-gel-type anion exchanger. Experimental results reveal that the pore structure of the anion exchanger plays a pivotal role in ensuring similar separation behavior of plutonium and neptunium along the separation protocol. It is proven that plutonium-242 ((242)Pu) performs well as a tracer for monitoring the chemical yield of neptunium when using AG MP-1 M resin, whereby the difficulties in obtaining a reliable and practicable isotopic neptunium tracer are overcome. An important asset of the SI setup is the feasibility of processing up to 100 g of solid substrates using a small-sized (ca. 2 mL) column with chemical yields of neptunium and plutonium being ≥79%. Analytical results of three certified/standard reference materials and two solid samples from intercomparison exercises are in good agreement with the reference values at the 0.05 significance level. The overall on-column separation can be completed within 3.5 h for 10 g of soil samples. Most importantly, the anion-exchange mini-column suffices to be reused up to 10-fold with satisfactory chemical yields (>70%), as demanded in environmental monitoring and emergency scenarios, making the proposed automated assembly well-suited for unattended and high-throughput analysis.

  15. Absorption-Line Detections of $10^{5-6}$ K Gas in Spiral-Rich Groups of Galaxies

    CERN Document Server

    Stocke, J T; Danforth, C W; Syphers, D; Yamamoto, H; Shull, J M; Green, J C; Froning, C; Savage, B D; Wakker, B; Kim, T -S; Ryan-Weber, E V; Kacprzak, G G

    2014-01-01

    Using the Cosmic Origins Spectrograph (COS) on the Hubble Space Telescope (HST) the COS Science Team has conducted a high signal-to-noise survey of 14 bright QSOs. In a previous paper (Savage et al. 2014) these far-UV spectra were used to discover 14 "warm" ($T > 10^5$ K) absorbers using a combination of broad Ly\\alpha\\ and O VI absorptions. A reanalysis of a few of this new class of absorbers using slightly relaxed fitting criteria finds as many as 20 warm absorbers can be present in this sample. A shallow, wide spectroscopic galaxy redshift survey has been conducted around these sight lines to investigate the warm absorber environment, which is found to be spiral-rich galaxy groups or cluster outskirts with radial velocity dispersions of \\sigma_v = 250-750 km/s. While 2\\sigma\\ evidence is presented favoring the hypothesis that these absorptions are associated with the galaxy groups and not with the individual nearest galaxies, this evidence has considerable systematic uncertainties and so is not conclusive....

  16. A HIRES Detection of NA I D Absorption in the Spectrum of the QSO PKS 2020-370 Due to the Galaxy Klemola 31A

    Science.gov (United States)

    Junkkarinen, V. T.; Barlow, T. A.

    1994-12-01

    By using the Keck telescope and HIRES spectrograph we have detected Na I D absorption lines in the spectrum of the QSO PKS 2020-370 (V = 17.5, z = 1.048) due to the galaxy Klemola 31A (z = 0.0288). The PKS 2020-370 line of sight is near an apparent spiral arm only 20" from the nucleus of Klemola 31A which corresponds to 17 kpc (H_o = 50 km s(-1) Mpc(-1) ). The spectrum of PKS 2020-370 has strong Ca II absorption lines (W_λ ~ 350 m Angstroms \\ for the K line) at the galaxy redshift (Boksenberg et al, 1980, ApJ, 242, L145), but previous attempts to detect Na I have resulted in upper limits (Boisse et al. 1988, A&A, 191, 193, Womble, 1992, thesis UCSD). We observed PKS 2020-370 with HIRES in May 1994 at a resolution of 8 km s(-1) FWHM for a total of 90 minutes. The Na I D doublet is detected with a total W_λ for the Na I 5891.6 Angstroms \\ (vac) absorption line of about 160 m Angstroms . The absorption appears as two main velocity components separated by 23 km s(-1) . The optically thin estimate for N(Na I) = 1.0 times 10(12) cm(-2) gives an estimated N(Ca II)/N(Na I) = 5. This value suggests that the gas in Klemola 31A along the QSO line of sight is ``halo like''. Along ``disk like'' lines of sight where Ca is thought to be depleted onto grains in our Galaxy, the N(Ca II)/N(Na I) ratio is usually small (Ca II)/N(Na I) ratios when the line of sight intersects starlight at 25 mag per sq. arcsec (Womble, 1992 thesis UCSD). The PKS 2020-370 sightline is near the optical extent of Klemola 31A but the N(Ca II)/N(Na I) is consistent with the sightline passing through two clouds in the halo. This research has been supported in part by NASA NAS5--29293 and NAG5--1630.

  17. Absolute determination of charge-coupled device quantum detection efficiency using Si K-edge x-ray absorption fine structure

    Energy Technology Data Exchange (ETDEWEB)

    Dunn, J; Steel, A B

    2012-05-06

    We report a method to determine the quantum detection efficiency and the absorbing layers on a front-illuminated charge-coupled device (CCD). The CCD under study, as part of a crystal spectrometer, measures intense continuum x-ray emission from a picosecond laser-produced plasma and spectrally resolves the Si K-edge x-ray absorption fine structure features due to the electrode gate structure of the device. The CCD response across the Si K-edge shows a large discontinuity as well as a number of oscillations that are identified individually and uniquely from Si, SiO{sub 2}, and Si{sub 3}N{sub 4} layers. From the spectral analysis of the structure and K-edge discontinuity, the active layer thickness and the different absorbing layers thickness can be determined precisely. A precise CCD detection model from 0.2-10 keV can be deduced from this highly sensitive technique.

  18. Extraction and preconcentration of trace levels of cobalt using functionalized magnetic nanoparticles in a sequential injection lab-on-valve system with detection by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: An approach to performing extraction and preconcentration employing functionalized magnetic particles for the determination of cobalt in the sequential injection lab-on-valve system using detection by electrothermal atomic absorption spectrometry. Highlights: ► New SPE method for cobalt separation/preconcentration was reported. ► Functionalized magnetic nanoparticles were used as adsorbent. ► Extraction, elution, and detection procedures were performed in the LOV system. ► This automatic extraction technique provided a good platform for metal analysis. - Abstract: A new approach to performing extraction and preconcentration employing functionalized magnetic nanoparticles for the determination of trace metals is presented. Alumina-coated iron oxide nanoparticles were synthesized and used as the solid support. The nanoparticles were functionalized with sodium dodecyl sulfate and used as adsorbents for solid phase extraction of the analyte. Extraction, elution, and detection procedures were performed sequentially in the sequential injection lab-on-valve (SI-LOV) system followed by electrothermal atomic absorption spectrometry (ETAAS). Mixtures of hydrophobic analytes were successfully extracted from solution using the synthesized magnetic adsorbents. The potential use of the established scheme was demonstrated by taking cobalt as a model analyte. Under the optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 0.01–5 μg L−1, and the relative standard deviation was 2.8% at the 0.5 μg L−1 level (n = 11). The limit of detection was 6 ng L−1 with a sampling frequency of 18 h−1. The present method has been successfully applied to cobalt determination in water samples and two certified reference materials.

  19. [Detection of common determinants of HLA antigens A2 and B17 by absorption using human HLA serum].

    Science.gov (United States)

    Májský, A; Korínková, P

    1983-01-01

    Attempts of cross absorption where sera of anti-HLA A2 + B17, anti-HLA A2 and anti-HLA B17 with thrombocytes were absorbed from donors of HLA A2 positive, B17 negative and HLA A2 negative, B17 positive, revealed that anti-HLA A2 and anti-HLA B17 could be eliminated from the sera of both HLA types on the platelets. Thus, the findings allow the existence of a common determinant of HLA A2 and B17-antigens to be assumed. This is the first case where the evidence of a cross reaction between antigens of two different HLA loci with human sera could be established.

  20. Extraction-mass spectrometric determination of platinum metals in materials of complex composition

    International Nuclear Information System (INIS)

    A method is developed for the extraction mass-spectrometric determination of platinum metals, including ruthenium. The loWer limit of detectable contents is 1.6x10-6 mass.% (a coefficient of concentration is 50). The relative standard deviation is 0.19-0.38. Relative sensitivity coefficients determined experimentally with the aid of reference samples for platinum metals enable the systematic errors of analysis results to be taken into account. The method is most advisably used for the simultaneous determination of platinum metals in complex objects (minerals, rocks, etc.)

  1. Water vapour emission in vegetable fuel: absorption cell measurements and detection limits of our CO II Dial system

    Science.gov (United States)

    Bellecci, C.; De Leo, L.; Gaudio, P.; Gelfusa, M.; Lo Feudo, T.; Martellucci, S.; Richetta, M.

    2006-09-01

    Forest fires can be the cause of serious environmental and economic damages. For this reason a considerable effort has been directed toward the forest protection and fire fighting. In the early forest fire detection, Lidar technique present considerable advantages compared to the passive detection methods based on infrared cameras currently in common use, due its higher sensitivity and ability to accurately locate the fire. The combustion phase of the vegetable matter causes a great amount of water vapour emission, thus the water molecule behaviour will be studied to obtain a fire detection system ready and efficient also before the flame propagation. A first evaluation of increment of the water vapour concentration compared to standard one will be estimated by a numerical simulation. These results will be compared with the experimental measurements carried out into a cell with a CO II Dial system, burning different kinds of vegetable fuel. Our results and their comparison will be reported in this paper.

  2. Comparison of Tunable Diode Laser Absorption Spectroscopy and Isothermal Micro-calorimetry for Non-invasive Detection of Microbial Growth in Media Fills

    Science.gov (United States)

    Brueckner, David; Roesti, David; Zuber, Ulrich Georg; Schmidt, Rainer; Kraehenbuehl, Stefan; Bonkat, Gernot; Braissant, Olivier

    2016-01-01

    Two methods were investigated for non-invasive microbial growth-detection in intact glass vials as possible techniques for automated inspection of media-filled units. Tunable diode laser absorption spectroscopy (TDLAS) was used to determine microbially induced changes in O2 and CO2 concentrations within the vial headspaces. Isothermal microcalorimetry (IMC) allowed the detection of metabolic heat production. Bacillus subtilis and Streptococcus salivarius were chosen as test organisms. Parameters as robustness, sensitivity, comparability and time to detection (TtD) were evaluated to assess method adequacy. Both methods robustly detected growth of the tested microorganisms within less than 76 hours using an initial inoculum of IMC, as some false negative results were observed. Compared to the visual media-fill examination of spiked samples, the investigated techniques were slightly slower regarding TtD. Although IMC showed shorter TtD than TDLAS the latter is proposed for automating the media-fill inspection, as larger throughput can be achieved. For routine use either TDLA or a combination of TDLA and TDLA should be considered. IMC may be helpful for replacing the sterility assessment of commercial drug products before release. PMID:27282661

  3. Analysis of Marine Biotoxins by Liquid Chromatography Mass Spectrometric Detection

    NARCIS (Netherlands)

    Gerssen, A.

    2014-01-01

    The last few years have brought about many changes in the field of marine and freshwater toxins, with advances in analytical technology and the realization that these toxins are a global issue. Offering a complete reference guide, Seafood and Freshwater Toxins: Pharmacology, Physiology, and Detectio

  4. Detection of Candida albicans by mass spectrometric fingerprinting.

    Science.gov (United States)

    Zehm, Sarah; Schweinitz, Simone; Würzner, Reinhard; Colvin, Hans Peter; Rieder, Josef

    2012-03-01

    Candida albicans is one of the most frequent causes of fungal infections in humans. Significant correlation between candiduria and invasive candidiasis has previously been described. The existing diagnostic methods are often time-consuming, cost-intensive and lack in sensitivity and specificity. In this study, the profile of low-molecular weight volatile compounds in the headspace of C. albicans-urine suspensions of four different fungal cell concentrations compared to nutrient media and urine without C. albicans was determined using proton-transfer reaction mass spectrometry (PTR-MS). At fungal counts of ≥1.5 × 10(5) colony forming units (CFU)/ml signals at 45, 47 and 73 atomic mass units (amu) highly significantly increased. At fungal counts of albicans-urine suspensions of different fungal cell concentrations. PTR-MS represents a promising approach to rapid, highly sensitive and non-invasive clinical diagnostics allowing qualitative and quantitative analysis.

  5. Mass Spectrometric Approaches to Detecting and Quantifying Prions

    Science.gov (United States)

    Prions are infectious proteins that replicate by converting a normal cellular protein (PrPC)into a prion. Although prions and PrPC are isoforms, they have dramatically different physicochemical properties. Prions are resistant to proteinase K (PK) degradation, while PrPC is completely degraded by PK...

  6. Study of the spectrometric performances of monolithic CdTe CdZnTe gamma ray detectors

    OpenAIRE

    Gros D'Aillon, Eric

    2005-01-01

    Pixelated monolithic CdTe / CdZnTe semiconductor gamma ray detectors are brought to replace scintillation detectors for medical applications, notably for single photon emission computed tomography (SPECT). In addition to compactness, they present better spectrometric performances: energy resolution, detection efficiency, and spatial resolution. Moreover, the photons depth of interaction in the crystal can be measured. This work aimed in studying experimentally and by simulation the correlatio...

  7. In Situ Probing of Cholesterol in Astrocytes at the Single Cell Level using Laser Desorption Ionization Mass Spectrometric Imaging with Colloidal Silver

    Energy Technology Data Exchange (ETDEWEB)

    Perdian, D.C.; Cha, Sangwon; Oh, Jisun; Sakaguchi, Donald S.; Yeung, Edward S.; and Lee, Young Jin

    2010-03-18

    Mass spectrometric imaging has been utilized to localize individual astrocytes and to obtain cholesterol populations at the single-cell level in laser desorption ionization (LDI) with colloidal silver. The silver ion adduct of membrane-bound cholesterol was monitored to detect individual cells. Good correlation between mass spectrometric and optical images at different cell densities indicates the ability to perform single-cell studies of cholesterol abundance. The feasibility of quantification is confirmed by the agreement between the LDI-MS ion signals and the results from a traditional enzymatic fluorometric assay. We propose that this approach could be an effective tool to study chemical populations at the cellular level.

  8. Detected CFCs: UV Absorption Spectra, Atmospheric Lifetimes, Global Warming and Ozone Depletion Potentials for CFC-112, CFC-112a, CFC-113a and CFC-114a

    Science.gov (United States)

    Bernard, F.; Davis, M. E.; McGillen, M.; Fleming, E. L.; Burkholder, J. B.

    2015-12-01

    Chlorofluorocarbons (CFCs) are ozone depleting substances (ODSs) and potent greenhouse gases. Measurements have observed CFC-112 (CFCl2CFCl2), CFC-112a (CF2ClCCl3), and CFC-113a (CCl3CF3) in the atmosphere (Laube et al., 2014). The current atmospheric abundances of CFC-112 and CFC-112a are ~0.4 and ~0.06 ppt, respectively, with decreasing abundance since 1995. In contrast, CFC-113a was found to show continuous growth over the past 50 years with a current atmospheric abundance of ~0.5 ppt. The major atmospheric removal process for these compounds is expected to be UV photolysis in the stratosphere. To date there is, however, no UV absorption spectra for these compounds available in the literature. To better determine the atmospheric lifetimes and environmental impact of these CFCs, laboratory measurements of the UV absorption spectra of CFC-112, CFC-112a, CFC-113a, and CFC-114a (Cl2FCF3) between 195 and 235 nm and over the temperature range 207 to 323 K were performed. Spectrum parametrizations were developed for use in atmospheric models. Atmospheric lifetimes and ozone depletion potentials (ODPs) were calculated using the Goddard Space Flight Center 2-D atmospheric chemistry model. Infrared absorption spectra of these compounds were also measured and used to calculate their global warming potentials. The results of the laboratory measurements and model calculations will be presented. J. C. Laube et al., Newly detected ozone-depleting substances in the atmosphere, Nature Geoscience, 7, 266-269, 2014

  9. Errarum: Detection of Absorption-Line Features in the X-Ray Spectra of the Galactic Superluminal Source GRO J1655-40

    Science.gov (United States)

    Ueda, Y.; Inoue, H.; Tanaka, Y.; Ebisawa, K.; Nagase, F.; Kotani, T.; Gehrels, N.

    1998-06-01

    In the paper ``Detection of Absorption-Line Features in the X-Ray Spectra of the Galactic Superluminal Source GRO J1655-40'' by Y. Ueda, H. Inoue, Y. Tanaka, K. Ebisawa, F. Nagase, T. Kotani, and N. Gehrels (ApJ, 492, 782 [1998]), there is an error in the curve of growth for the Kα absorption line (Fig. 4). The revised version of Figure 4 given here replaces Figure 4 in the paper. Several numbers derived from the figure should be corrected accordingly, but the conclusion of the paper is not affected. In the third paragraph of the discussion section (page 786), the iron column density of the plasma should be 1019-1020 cm-2, which corresponds to a hydrogen column density of 3 × 1023-3 × 1024 cm-2. The final limit on the hydrogen column density of the line-absorbing plasma should be changed to 3 × 1023 cm-2 < NH < 1024 cm-2.

  10. Detection of para–antiferromagnetic transition in Bi{sub 2}Fe{sub 4}O{sub 9} powders by means of microwave absorption measurements

    Energy Technology Data Exchange (ETDEWEB)

    Alvarez, G., E-mail: memodin@yahoo.com [Escuela Superior de Física y Matemáticas del Instituto Politécnico Nacional, U.P.A.L.M, Edificio 9, Av. Instituto Politécnico Nacional S/N, San Pedro Zacatenco, México DF 07738 (Mexico); Contreras, J. [Facultad de Química de la Universidad Nacional Autónoma de México, Cd. Universitaria, México DF 04510 (Mexico); Conde-Gallardo, A. [Departamento de Física, CINVESTAV-IPN, A.P. 14-740, México DF 07360 (Mexico); Montiel, H., E-mail: herlinda_m@yahoo.com [Centro de Ciencias Aplicadas y Desarrollo Tecnológico de la Universidad Nacional Autónoma de México, Cd. Universitaria, A.P. 70-186, México DF 04510 (Mexico); Zamorano, R. [Escuela Superior de Física y Matemáticas del Instituto Politécnico Nacional, U.P.A.L.M, Edificio 9, Av. Instituto Politécnico Nacional S/N, San Pedro Zacatenco, México DF 07738 (Mexico)

    2013-12-15

    An electron paramagnetic resonance (EPR) study of Bi{sub 2}Fe{sub 4}O{sub 9} powders is carried out in X-band (8.8–9.8 GHz) and the 200–350 K temperature range. For all the temperatures, the EPR spectra show a single broad line attributable to Fe{sup 3+} (S=5/2) ions. The onset of the para–antiferromagnetic transition has been determined from the temperature dependence of the parameters deduced from EPR spectra: the peak-to-peak linewidth (ΔH{sub pp}) and the resonant field (H{sub res}); a weak ferromagnetism is also observed at low temperature and it is attributed to canting of Fe{sup 3+} ion sublattices in the antiferromagnetic matrix. The magnetically modulated microwave absorption spectroscopy (MAMMAS) and the low-field microwave absorption (LFMA) are used to give further information on this material. These techniques give evidence of the magnetic transition, suggesting a weak ferromagnetism at low temperature. - Highlights: • The changes in lineshape of the EPR spectra in Bi{sub 2}Fe{sub 4}O{sub 9} powders are studied. • The onset of the para–antiferromagnetic transition is detected. • A weak ferromagnetism is also observed in this material. • MAMMAS and LFMA techniques are used to give a further knowledge on the bismuth ferrite.

  11. Novel Fiber Optic Sensor Probe with a Pair of Highly Reflected Connectors and a Vessel of Water Absorption Material for Water Leak Detection

    Science.gov (United States)

    Cho, Tae-Sik; Choi, Ki-Sun; Seo, Dae-Cheol; Kwon, Il-Bum; Lee, Jung-Ryul

    2012-01-01

    The use of a fiber optic quasi-distributed sensing technique for detecting the location and severity of water leakage is suggested. A novel fiber optic sensor probe is devised with a vessel of water absorption material called as water combination soil (WCS) located between two highly reflected connectors: one is a reference connector and the other is a sensing connector. In this study, the sensing output is calculated from the reflected light signals of the two connectors. The first reflected light signal is a reference and the second is a sensing signal which is attenuated by the optical fiber bending loss due to the WCS expansion absorbing water. Also, the bending loss of each sensor probe is determined by referring to the total number of sensor probes and the total power budget of an entire system. We have investigated several probe characteristics to show the design feasibility of the novel fiber sensor probe. The effects of vessel sizes of the probes on the water detection sensitivity are studied. The largest vessel probe provides the highest sensitivity of 0.267 dB/mL, while the smallest shows relatively low sensitivity of 0.067 dB/mL, and unstable response. The sensor probe with a high output value provides a high sensitivity with various detection levels while the number of total installable sensor probes decreases. PMID:23112637

  12. Researchon Optical Fiber Hydrogen Sulfide Gas Detection with Absorption Spectrum%吸收型光纤硫化氢气体检测研究

    Institute of Scientific and Technical Information of China (English)

    贾振安; 王俊锋; 周红; 白亮; 王炜

    2013-01-01

    Based on the theory of selective absorption of gas in the near-infrared region and the Beer-Lambert law,Raman scattering characteristics of hydrogen sulfide gas are researched.Meanwhile,a broad-band light source is used to detect the concentration of H2S gas.Self-focusing lenses are used as collimating or focusing lens for transmission gas cell.A method using cascaded GRIN lens to increase the optical-path length is presented,and the detection sensitivity of the gas cell is greatly increased by this method.By analyzing the experimental curves of hydrogen sulfide absorption,it is shown that the system sensitivity is 3.672× 10 4 μW/(μL/L),and the resolution is 122.5 μL/L.%基于气体近红外选择性吸收理论和Beer-Lambert定律,研究了硫化氢气体的拉曼散射特性,同时采用宽带光源光谱吸收检测技术对H2S气体进行检测.将自聚焦透镜作为光纤准直透镜和聚焦透镜,并将其应用于透射型气室.同时,提出了在透射式气室中将多对自聚焦透镜组串联使用以增加吸收光程的方法,该方法可以明显提高气室的检测灵敏度.通过分析实验测得的H2S吸收曲线,得到系统的灵敏度为3.672×10-4 μW/(μL/L),分辨率为122.5 μL/L.

  13. Aeromagnetic and gamma spectrometric interpretation of the Riacho Queimadas sheet

    International Nuclear Information System (INIS)

    This paper presents the aeromagnetic and gamma-spectrometric interpretation of the Riacho Queimadas Sheet (SC.24-V-A-I), southeastern Piaui State, Brazil, originated from studies as part of the Programa Levantamentos Geologicos Basicos do Brasil-PLGB (basic Geological Surveying Program of Brazil). The interpretation of magnetometric and gamma-spectrometric maps identified mafic-ultramafic and felsic terrains and sedimentary rocks and the utilization of modelling techniques defined the shape and variation in thickness of geologic bodies. It was possible to limit young igneous intrusive rocks and to suggest the hierarchy of structural alignments and shear zones, based on anomalies shape analyses. (author)

  14. Experimental characterization of the Clear-PEM scanner spectrometric performance

    Science.gov (United States)

    Bugalho, R.; Carriço, B.; Ferreira, C. S.; Frade, M.; Ferreira, M.; Moura, R.; Ortigão, C.; Pinheiro, J. F.; Rodrigues, P.; Rolo, I.; Silva, J. C.; Trindade, A.; Varela, J.

    2009-10-01

    In the framework of the Clear-PEM project for the construction of a high-resolution and high-specificity scanner for breast cancer imaging, a Positron Emission Mammography tomograph has been developed and installed at the Instituto Português de Oncologia do Porto hospital. The Clear-PEM scanner is mainly composed by two planar detector heads attached to a robotic arm, trigger/data acquisition electronics system and computing servers. The detector heads hold crystal matrices built from 2 × 2 × 20 mm3 LYSO:Ce crystals readout by Hamamatsu S8550 APD arrays. The APDs are optically coupled to both ends of the 6144 crystals in order to extract the DOI information for each detected event. Each one of 12288 APD's pixels is read and controlled by Application Specific Integrated Circuits water-cooled by an external cooling unit. The Clear-PEM frontend boards innovative design results in a unprecedented integration of the crystal matrices, APDs and ASICs, making Clear-PEM the PET scanner with the highest number of APD pixels ever integrated so far. In this paper, the scanner's main technical characteristics, calibration strategies and the first spectrometric performance evaluation in a clinical environment are presented. The first commissioning results show 99.7% active channels, which, after calibration, have inter-pixel and absolute gain distributions with dispersions of, respectively, 12.2% and 15.3%, demonstrating that despite the large number of channels, the system is uniform. The mean energy resolution at 511 keV is of 15.9%, with a 8.8% dispersion, and the mean CDOI-1 is 5.9%/mm, with a 7.8% dispersion. The coincidence time resolution, at 511 keV, for a energy window between 400 and 600 keV, is 5.2 ns FWHM.

  15. Detection and diagnosis of a natural gas dehydration plant by absorption with triethylene glycol, employing a artificial neural networks

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2004-07-01

    The natural gas dehydration is a great importance operation in the gas and petroleum industry, It avoids operational problems associated with the water content, which appear frequently in the industrial facilities that use the natural gas as raw material or as work tool. Due to the presence of undesirable pollutants which may enter the plant with the wet natural gas current (lubricating, corrosion inhibitors, salts, and others), the equipment that constitutes the dehydration plants are capable to suffering operational faults as the heat exchangers fouling, foam formation in the absorber, glycol losses for dragging; trays, packings, valves and filters fouling; glycol degradation, inadequate temperatures of regeneration and others. The above mentioned faults often cannot be detected by the operators and engineers but up to the moment when a catastrophic damage occurs or when products are obtained out of specification, which causes big economic and time losses. By means of the application of artificial neural networks, there was achieved the detection and the effective diagnosis of faults, still in incipient state, in a gas dehydration plant. (author)

  16. Analysis of Polar Lipids in Chlamydomonas reinhardtii Using Nanoelectrospray Direct Infusion Method and Gas Chromatography and Mass Spectrometric Detection%基于芯片的直接进样质谱法和气相色谱-质谱测定莱茵衣藻中的极性脂类

    Institute of Scientific and Technical Information of China (English)

    杨大伟; 范晓蕾; Kind Tobias; Fiehn Oliver; 郭荣波

    2013-01-01

    . reinhardtii. Among them, twenty classes of diacylglyceryltrimethylhomoserine that are very special lipid species in C. reinhardtii belonging to betaine lipids were annotated with in-house Lipidblast database. In order to validate this Lipidblast match, we performed a manual spectral interpretation of every experimental MS/MS spectrum to ensure authentic ester annotations. Besides, we also applied a gas chromatography tandem mass spectrometric method to detect free fatty acids in C. reinhardtii and found that linolenic acid, linoleic acid and palmitic acid are most abundant free fatty acids in C. reinhardtii. This study provides a potential comprehensive lipidomic method for further lipid analysis in algal research.

  17. Ultrasound-assisted emulsification of cosmetic samples prior to elemental analysis by different atomic spectrometric techniques.

    Science.gov (United States)

    Lavilla, I; Cabaleiro, N; Costas, M; de la Calle, I; Bendicho, C

    2009-11-15

    In this work, ultrasound-assisted emulsification with a probe system is proposed as a rapid and simple sample treatment for atomic spectrometric determinations (Electrothermal Atomic Absorption Spectrometry, Inductively Coupled Plasma Optical Emission Spectrometry, Flame Atomic Absorption Spectrometry and Cold Vapour Atomic Absorption Spectrometry) of trace elements (As, Cd, Cr, Cu, Hg, Mg, Mn, Ni, Sr and Zn) in cosmetic samples such as shampoos, gel (hair gel), crèmes (body milk, hair conditioner) and oil (body oil). The type of dispersion medium, the sample mass-to-dispersion medium volume ratio, as well as the parameters related to the ultrasound-assisted emulsification (sonication amplitude and treatment time) were exhaustively studied. Only 1 min of ultrasonic shaking and a dispersion medium containing 0.5% (w/v) of SDS+3% (v/v) of HNO(3) or HCl allows obtaining a stable emulsion at least for 3 months. Thermal programs, nebulization of emulsions, speed of pumps and concentration of reagents used in cold vapour generation were optimized. Calibration using aqueous standards was feasible in all cases. Calibration by the standard addition method and recovery studies was also applied for validation. Microwave-assisted digestion and Inductively Coupled Plasma Mass Spectrometry were used for comparison purposes. Relative standard deviations from analysis of five independent emulsions were less than 9% in all cases. PMID:19782199

  18. Simultaneous detection of the absorption spectrum and refractive index ratio with a spectrophotometer: monitoring contaminants in bioethanol

    Science.gov (United States)

    Kontturi, V.; Hyvärinen, S.; García, A.; Carmona, R.; Murzin, D. Yu; Mikkola, J.-P.; Peiponen, K.-E.

    2011-05-01

    The optical properties of a biofuel resulting from the fungi-treated lignocellulosic biomass in an ethanol matrix were studied. The matrix simulates the case that the bioethanol is contaminated by sugars, water and colour pigments that reduce the quality of the biofuel and compromise the combustion process. It is suggested that by applying a spectrophotometer only, it is possible to obtain valid information, i.e. the spectral features of the contaminants as well as the refractive index ratio of bioethanol. This allows for simultaneous purity and density detection of biomass-derived liquids or liquid biofuels, in comparison to a reference representing an ideal bioethanol (pure ethyl alcohol, ethanol of 99.5% purity (v/v)).

  19. Coumarin-based fluorescence hybrid silica material used for selective detection and absorption of Hg2+ in aqueous media

    Science.gov (United States)

    Meng, Qingtao; Jia, Hongmin; Wang, Cuiping; Zhao, Hongbin; Lu, Gonghao; Hu, Zhizhi; Zhang, Zhiqiang; Duan, Chunying

    2014-11-01

    An inorganic-organic hybrid fluorescence material (C-SBA-15) was prepared by covalent immobilization of a coumarin derivative within the channels of SBA-15. The characterization results of XRD, TEM micrographs, FT-IR and UV-vis demonstrate that coumarin is successfully grafted onto the inner surface of SBA-15 and its organized structure is preserved. C-SBA-15 can detect Hg2+ with high selectivity to Pb2+, Zn2+, Cu2+, Mn2+, Cd2+, Co2+, Ag+, Fe3+, Ni2+, K+, Na+, Ca2+, Mg2+ and Li+ in water. Furthermore, the fluorogenical response is reversible by treating with EDTA and do not vary over a broad pH range (5.0-10.5). C-SBA-15 features more outstanding absorbing capacity for Hg2+ among other HTM ions in water.

  20. Study of the spectrometric performances of monolithic CdZnTe / CdTe gamma ray detectors

    International Nuclear Information System (INIS)

    Pixelated monolithic CdTe/CdZnTe semiconductor gamma ray detectors are brought to replace scintillation detectors for medical applications, notably for single photon emission computed tomography (SPECT). In addition to compactness, they present better spectrometric performances: energy resolution, detection efficiency, and spatial resolution. Moreover, the photons depth of interaction in the crystal can be measured. This work aimed in studying experimentally and by simulation the correlations between anodes pitch, material physic properties (resistivity and electron transport properties), and detectors spectrometric performances. We have compared several methods of measuring the photon interaction depth, and have obtained an energy resolution ranging from 1.7% to 7% at 122 keV, according to material, for 5 mm thick detectors. Charge sharing between adjacent anodes has been studied and a measured data processing is proposed. (author)

  1. Standard test methods for chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide (Gd2O3) powder

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 These test methods cover procedures for the chemical and mass spectrometric analysis of nuclear-grade gadolinium oxide powders to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Carbon by Direct CombustionThermal Conductivity C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Total Chlorine and Fluorine by Pyrohydrolysis Ion Selective Electrode C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Loss of Weight on Ignition 7-13 Sulfur by CombustionIodometric Titration Impurity Elements by a Spark-Source Mass Spectrographic C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical,Nuclear, and Radiochemical Analysis of Uranium Hexafluoride C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry Gadolinium Content in Gadolinium Oxid...

  2. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    International Nuclear Information System (INIS)

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  3. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  4. Infrared differential-absorption Mueller matrix spectroscopy and neural network-based data fusion for biological aerosol standoff detection.

    Science.gov (United States)

    Carrieri, Arthur H; Copper, Jack; Owens, David J; Roese, Erik S; Bottiger, Jerold R; Everly, Robert D; Hung, Kevin C

    2010-01-20

    An active spectrophotopolarimeter sensor and support system were developed for a military/civilian defense feasibility study concerning the identification and standoff detection of biological aerosols. Plumes of warfare agent surrogates gamma-irradiated Bacillus subtilis and chicken egg white albumen (analytes), Arizona road dust (terrestrial interferent), water mist (atmospheric interferent), and talcum powders (experiment controls) were dispersed inside windowless chambers and interrogated by multiple CO(2) laser beams spanning 9.1-12.0 microm wavelengths (lambda). Molecular vibration and vibration-rotation activities by the subject analyte are fundamentally strong within this "fingerprint" middle infrared spectral region. Distinct polarization-modulations of incident irradiance and backscatter radiance of tuned beams generate the Mueller matrix (M) of subject aerosol. Strings of all 15 normalized elements {M(ij)(lambda)/M(11)(lambda)}, which completely describe physical and geometric attributes of the aerosol particles, are input fields for training hybrid Kohonen self-organizing map feed-forward artificial neural networks (ANNs). The properly trained and validated ANN model performs pattern recognition and type-classification tasks via internal mappings. A typical ANN that mathematically clusters analyte, interferent, and control aerosols with nil overlap of species is illustrated, including sensitivity analysis of performance. PMID:20090802

  5. Active Stand-off Detection of Gas Leaks Using a Short Range Hard-target Backscatter Differential Optical Absorption System Based on a Quantum Cascade Laser Transmitter

    Science.gov (United States)

    Diaz, Adrian; Thomas, Benjamin; Castillo, Paulo; Gross, Barry; Moshary, Fred

    2016-06-01

    Fugitive gas emissions from agricultural or industrial plants and gas pipelines are an important environmental concern as they can contribute to the global increase of greenhouse gas concentration. Moreover, they are also a security and safety concern because of possible risk of fire/explosion or toxicity. This study presents gas concentration measurements using a quantum cascade laser open path system (QCLOPS). The system retrieves the pathaveraged concentration of N2O and CH4 by collecting the backscattered light from a scattering target. The gas concentration measurements have a high temporal resolution (68 ms) and are achieved at sufficient range (up to 40 m, ~ 130 feet) with a detection limit of 2.6 ppm CH4 and 0.4 ppm for N2O. Given these characteristics, this system is promising for mobile/multidirectional remote detection and evaluation of gas leaks. The instrument is monostatic with a tunable QCL emitting at ~ 7.7 μm wavelength range. The backscattered radiation is collected by a Newtonian telescope and focused on an infrared light detector. Puffs of N2O and CH4 are released along the optical path to simulate a gas leak. The measured absorption spectrum is obtained using the thermal intra-pulse frequency chirped DFB QCL and is analyzed to obtain path averaged gas concentrations.

  6. Recent advances in mass spectrometric applications in hydrology

    International Nuclear Information System (INIS)

    The recent advances in mass spectrometric applications in hydrology include 18O of nitrates and sulphates, 37Cl of chlorides for studying origin of groundwater pollution, 3He/4He for geothermal fluids and analysis, 14C, 36Cl and 129I for dating groundwater by Accelerator Mass Spectrometry (AMS)

  7. Preparation and spectrometric identification of amide derivatives with antimalaric

    International Nuclear Information System (INIS)

    The structures of polymeric compounds using spectrometric analysis of infrared, ultraviolet and protonic magnetic resonance and 13C nuclear magnetic resonance are studied. Some structural models are used such as antimalaric-sulfones and pyrimidinic derivatives, and non-polymeric derivatives of active compounds. A comparative analysis on structures less complexes is shown. (M.J.C.). Spectrums 186 p

  8. Absorption-line detections of 10{sup 5}-10{sup 6} K gas in spiral-rich groups of galaxies

    Energy Technology Data Exchange (ETDEWEB)

    Stocke, John T.; Keeney, Brian A.; Danforth, Charles W.; Syphers, David; Yamamoto, H.; Shull, J. Michael; Green, James C.; Froning, Cynthia [Center for Astrophysics and Space Astronomy, Department of Astrophysical and Planetary Sciences, University of Colorado, 389 UCB, Boulder, CO 80309 (United States); Savage, Blair D.; Wakker, Bart; Kim, Tae-Sun [Department of Astronomy, University of Wisconsin, Madison, WI 53706 (United States); Ryan-Weber, Emma V.; Kacprzak, Glenn G., E-mail: john.stocke@colorado.edu [Centre for Astrophysics and Supercomputing, Swinburne University of Technology, VIC 3122 (Australia)

    2014-08-20

    Using the Cosmic Origins Spectrograph (COS) on the Hubble Space Telescope, the COS Science Team has conducted a high signal-to-noise survey of 14 bright QSOs. In a previous paper, these far-UV spectra were used to discover 14 'warm' (T ≥ 10{sup 5} K) absorbers using a combination of broad Lyα and broad O VI absorptions. A reanalysis of a few of this new class of absorbers using slightly relaxed fitting criteria finds as many as 20 warm absorbers could be present in this sample. A shallow, wide spectroscopic galaxy redshift survey has been conducted around these sight lines to investigate the warm absorber environment, which is found to be spiral-rich groups or cluster outskirts with radial velocity dispersions σ = 250-750 km s{sup –1}. While 2σ evidence is presented favoring the hypothesis that these absorptions are associated with the galaxy groups and not with the individual, nearest galaxies, this evidence has considerable systematic uncertainties and is based on a small sample size so it is not entirely conclusive. If the associations are with galaxy groups, the observed frequency of warm absorbers (dN/dz = 3.5-5 per unit redshift) requires them to be very extended as an ensemble on the sky (∼1 Mpc in radius at high covering factor). Most likely these warm absorbers are interface gas clouds whose presence implies the existence of a hotter (T ∼ 10{sup 6.5} K), diffuse, and probably very massive (>10{sup 11} M {sub ☉}) intra-group medium which has yet to be detected directly.

  9. Redox speciation analysis of dissolved iron in estuarine and coastal waters with on-line solid phase extraction and graphite furnace atomic absorption spectrometry detection.

    Science.gov (United States)

    Chen, Yaojin; Feng, Sichao; Huang, Yongming; Yuan, Dongxing

    2015-05-01

    An automatic on-line solid phase extraction (SPE) system employing the flow injection (FI) technique directly coupled to a graphite furnace atomic absorption spectrometer (GFAAS) was established for speciation and determination of dissolved iron in estuarine and coastal waters. Fe(II) was mixed with ferrozine solution in a sample stream to form the Fe(II)-ferrozine complex which was extracted onto a C18 SPE cartridge, eluted with eluent and detected with GFAAS. In a parallel flow channel, Fe(III) was reduced to Fe(II) with ascorbic acid and then detected in the same way as Fe(II). The home-made interface between FI-SPE and GFAAS efficiently realized the sample introduction to the furnace in a semi-automated way. Parameters of the FI-SPE system and graphite furnace program were optimized based on a univariate experimental design and an orthogonal array design. The salinity effect on the method sensitivity was investigated. The proposed method provided a detection limit of 1.38 nmol L(-1) for Fe(II) and 1.87 nmol L(-1) for Fe(II+III). With variation of the sample loading volume, a broadened determination range of 2.5-200 nmol L(-1) iron could be obtained. The proposed method was successfully applied to analyze iron species in samples collected from the Jiulongjiang Estuary, Fujian, China. With the 2-cartridge FI-SPE system developed, on-line simultaneous determination of Fe species with GFAAS was achieved for the first time. PMID:25770602

  10. The Bremen mass spectrometric facility for the measurement of helium isotopes, neon, and tritium in water.

    Science.gov (United States)

    Sültenfuss, Jürgen; Roether, Wolfgang; Rhein, Monika

    2009-06-01

    We describe the mass spectrometric facility for measuring helium isotopes, neon, and tritium that has been operative at this institute since 1989, and also the sampling and sample preparation steps that precede the mass spectrometric analysis. For water samples in a near-equilibrium with atmospheric air, the facility achieves precision for (3)He/(4)He ratios of+/-0.4% or better, and+/-0.8 % or better for helium and neon concentrations. Tritium precision is typically+/-3 % and the detection limit 10 mTU ( approximately 1.2.10(-3) Bq/kg of pure water). Sample throughputs can reach some thousands per year. These achievements are enabled, among other features, by automation of the measurement procedure and by elaborate calibration, assisted by continual development in detail. To date, we have measured more than 15,000 samples for tritium and 23,000 for helium isotopes and neon, mostly in the context of oceanographic and hydrologic work. Some results of such work are outlined. Even when atmospheric tritium concentrations have become rather uniform, tritium provides water ages if (3)He data are taken concurrently. The technique can resolve tritium concentrations in waters of the pre-nuclear era.

  11. Assessment of current mass spectrometric workflows for the quantification of low abundant proteins and phosphorylation sites

    Directory of Open Access Journals (Sweden)

    Manuel Bauer

    2015-12-01

    Full Text Available The data described here provide a systematic performance evaluation of popular data-dependent (DDA and independent (DIA mass spectrometric (MS workflows currently used in quantitative proteomics. We assessed the limits of identification, quantification and detection for each method by analyzing a dilution series of 20 unmodified and 10 phosphorylated synthetic heavy labeled reference peptides, respectively, covering six orders of magnitude in peptide concentration with and without a complex human cell digest background. We found that all methods performed very similarly in the absence of background proteins, however, when analyzing whole cell lysates, targeted methods were at least 5–10 times more sensitive than directed or DDA methods. In particular, higher stage fragmentation (MS3 of the neutral loss peak using a linear ion trap increased dynamic quantification range of some phosphopeptides up to 100-fold. We illustrate the power of this targeted MS3 approach for phosphopeptide monitoring by successfully quantifying 9 phosphorylation sites of the kinetochore and spindle assembly checkpoint component Mad1 over different cell cycle states from non-enriched pull-down samples. The data are associated to the research article ‘Evaluation of data-dependent and data-independent mass spectrometric workflows for sensitive quantification of proteins and phosphorylation sites׳ (Bauer et al., 2014 [1]. The mass spectrometry and the analysis dataset have been deposited to the ProteomeXchange Consortium (http://proteomecentral.proteomexchange.org via the PRIDE partner repository with the dataset identifier PXD000964.

  12. Time-resolved in situ detection of CO in a shock tube using cavity-enhanced absorption spectroscopy with a quantum-cascade laser near 4.6 µm.

    Science.gov (United States)

    Sun, Kai; Wang, Shengkai; Sur, Ritobrata; Chao, Xing; Jeffries, Jay B; Hanson, Ronald K

    2014-10-01

    Cavity-enhanced absorption spectroscopy (CEAS) using a mid-infrared DFB quantum-cascade laser is reported for sensitive time-resolved (10 μs) in situ CO measurements in a shock tube. Off-axis alignment and fast scanning of the laser wavelength were used to minimize coupling noise in a low-finesse cavity. An absorption gain factor of 91 was demonstrated, which enabled sub-ppm detection sensitivity for gas temperatures of 1000-2100K in a 15 cm diameter shock tube. This substantial improvement in detection sensitivity compared to conventional single-pass absorption measurements, shows great potential for the study of reaction pathways of high-temperature combustion kinetics mechanisms in shock tubes.

  13. Determination of Cd(II, Zn(II and Ag(Iin different matrixes after solid phase extraction on sodium dodecyl sulfate(SDS-coated alumina as their 2,3 Di Hydro 2,3 paratolylQinazoline (1 H- 4 one (DPTQO by Flame atomic absorption spectrometric

    Directory of Open Access Journals (Sweden)

    Farveh Raoufi

    2016-03-01

    Full Text Available A sensitive and selective solid phase extraction procedure for the determination of traces of Cd(II, Zn(II and Ag(I ions has been developed. An alumina-sodium dodecyl sulfate (SDS coated on with 2,3 Di Hydro 2,3 paratolylQinazoline (1 H- 4 one (DPTQO. The influences of the analytical parameters including pH and sample volume were investigated.Common coexisting ions did not interfere on the separation and determination of analytes under study. The adsorbed analytes were desorbed by using 6mL of 4 mol L−1 nitric acid. The responses are linear 0.02–0.85 µg mL-1 for Cd2+ ion0.01–0.90 µg mL-1 for Zn2+and0.02–0.92µg mL-1for Ag+ detection limit for Cd(II, Zn(II and Ag(I ions were found to be 1.4, 1.3 and1.12(ng mL-1, respectively.It was found that the recovery for Cd2+, Zn2+and Ag+ ions were 97.7, 98.2 and 98.0 with RSD of 1.9, 1.8 and 1.7. It was also observed that recovery for repeated recovery on the same solid phase not varies more than 3%. The presented procedurewas successfully applied for determination of analytes in radiology wastewater, amalgam, natural water and blood samples.

  14. Infrared Absorption Spectra, Radiative Efficiencies, and Global Warming Potentials of Newly-Detected Halogenated Compounds: CFC-113a, CFC-112 and HCFC-133a

    Directory of Open Access Journals (Sweden)

    Maryam Etminan

    2014-07-01

    Full Text Available CFC-113a (CF3CCl3, CFC-112 (CFCl2CFCl2 and HCFC-133a (CF3CH2Cl are three newly detected molecules in the atmosphere that are almost certainly emitted as a result of human activity. It is important to characterise the possible contribution of these gases to radiative forcing of climate change and also to provide information on the CO2-equivalence of their emissions. We report new laboratory measurements of absorption cross-sections of these three compounds at a resolution of 0.01 cm−1 for two temperatures 250 K and 295 K in the spectral range of 600–1730 cm−1. These spectra are then used to calculate the radiative efficiencies and global warming potentials (GWP. The radiative efficiencies are found to be between 0.15 and 0.3 W∙m−2∙ppbv−1. The GWP for a 100 year time horizon, relative to carbon dioxide, ranges from 340 for the relatively short-lived HCFC-133a to 3840 for the longer-lived CFC-112. At current (2012 concentrations, these gases make a trivial contribution to total radiative forcing; however, the concentrations of CFC-113a and HCFC-133a are continuing to increase. The 2012 CO2-equivalent emissions, using the GWP (100, are estimated to be about 4% of the current global CO2-equivalent emissions of HFC-134a.

  15. Determination of trace aluminum in biological and water samples by cloud point extraction preconcentration and graphite furnace atomic absorption spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Sang Hongbo [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Liang Pei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)], E-mail: liangpei@mail.ccnu.edu.cn; Du Dan [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)

    2008-06-15

    A cloud point extraction (CPE) method for the preconcentration of trace aluminum prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) has been developed. The CPE method is based on the complex of Al(III) with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP), and then entrapped in non-ionic surfactant Triton X-114. PMBP was used not only as chelating reagent in CPE preconcentration, but also as chemical modifier in GFAAS determination. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PMBP and Triton X-114, equilibration temperature and time, were investigated in detail. An enrichment factor of 37 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of this method for Al(III) is 0.09 ng mL{sup -1}, and the relative standard deviation is 4.7% at 10 ng mL{sup -1} Al(III) level (n = 7). The proposed method has been applied for determination of trace amount of aluminum in biological and water samples with satisfactory results.

  16. Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

    International Nuclear Information System (INIS)

    Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L−1 for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L−1, n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009–88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3–116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix. - Highlights: • Novel Cd(II)-II-MMS was prepared by surface imprinting combined with a sol–gel process. • Cd(II)-II-MMS has a high selectivity and adsorption capacity for Cd(II). • A sensitive and selective method of Cd(II)-IIMSPE-GFAAS was developed for trace cadmium analysis. • The method can be applied to determine trace Cd in various samples with complicated matrix

  17. Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Bingshan; He, Man; Chen, Beibei; Hu, Bin, E-mail: binhu@whu.edu.cn

    2015-05-01

    Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L{sup −1} for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L{sup −1}, n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009–88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3–116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix. - Highlights: • Novel Cd(II)-II-MMS was prepared by surface imprinting combined with a sol–gel process. • Cd(II)-II-MMS has a high selectivity and adsorption capacity for Cd(II). • A sensitive and selective method of Cd(II)-IIMSPE-GFAAS was developed for trace cadmium analysis. • The method can be applied to determine trace Cd in various samples with complicated matrix.

  18. A sensitive magnetic nanoparticle-based immunoassay of phosphorylated acetylcholinesterase using protein cage templated lead phosphate for signal amplification with graphite furnace atomic absorption spectrometry detection.

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Yang, Enjian; Ge, Xiaoxiao; Du, Dan; Lin, Yuehe

    2016-04-01

    We developed a new magnetic nanoparticle sandwich-like immunoassay using protein cage nanoparticles (PCN) for signal amplification together with graphite furnace atomic absorption spectrometry (GFAAS) for the quantification of an organophosphorylated acetylcholinesterase adduct (OP-AChE), the biomarker of exposure to organophosphate pesticides (OPs) and nerve agents. OP-AChE adducts were firstly captured by titanium dioxide coated magnetic nanoparticles (TiO2-MNPs) from the sample matrixes through metal chelation with phospho-moieties, and then selectively recognized by anti-AChE antibody labeled on PCN which was packed with lead phosphate in its cavity (PCN-anti-AChE). The sandwich-like immunoreaction was performed among TiO2-MNPs, OP-AChE and PCN-anti-AChE to form a TiO2-MNP/OP-AChE/PCN-anti-AChE immunocomplex. The complex could be easily isolated from the sample solution with the help of magnet, and the released lead ions from PCN were detected by GFAAS for the quantification of OP-AChE. Greatly enhanced sensitivity was achieved because PCN increased the amount of metal ions in the cavity of each apoferritin. The proposed immunoassay yielded a linear response over a broad range of OP-AChE concentrations from 0.01 nM to 2 nM, with a detection limit of 2 pM, which has enough sensitivity for monitoring of low-dose exposure to OPs. This new method showed an acceptable stability and reproducibility and was validated with OP-AChE spiked human plasma.

  19. Sensitive magnetic nanoparticle-based immunoassay of phosphorylated acetylcholinesterase using protein cage templated lead phosphate for signal amplification with graphite furnace atomic absorption spectrometry detection

    Science.gov (United States)

    Liang, Pei; Kang, Caiyan; Yang, Enjian; Ge, Xiaoxiao; Du, Dan; Lin, Yuehe

    2016-01-01

    We developed a new magnetic nanoparticles sandwich-like immunoassay using protein cage nanoparticles (PCN) for signal amplification together with graphite furnace atomic absorption spectrometry (GFAAS) for quantification of organophosphorylated acetylcholinesterase adduct (OP-AChE), the biomarker of exposure to organophosphate pesticides (OPs) and nerve agents. OP-AChE adducts were firstly captured by titanium dioxide coated magnetic nanoparticles (TiO2-MNPs) from the sample matrixes through metal chelation with phospho-moieties, and then selectively recognized by anti-AChE antibody labeled on PCN which was packed with lead phosphate in its cavity (PCN-anti-AChE). The sandwich-like immunoreaction was performed among TiO2-MNPs, OP-AChE and PCN-anti-AChE to form TiO2-MNPs/OP-AChE/PCN-anti-AChE immunocomplex. The complex could be easily isolated from the sample solution with the help of magnet, and the released lead ions from PCN were detected by GFAAS for the quantification of OP-AChE. Greatly enhanced sensitivity was achieved because PCN increased the amount of metal ions in the cavity of each apoferritin. The proposed immunoassay yielded a linear response over a broad OP-AChE concentrations from 0.01 nM to 2 nM, with a detection limit of 2 pM, which has enough sensitivity for monitoring of low-dose exposure to OPs. This new method showed an acceptable stability and reproducibility and was validated with OP-AChE spiked human plasma. PMID:26953358

  20. Development and Integration of a Pulsed 2-micron Direct Detection Integrated Path Differential Absorption (IPDA) Lidar for CO2 Column Measurement from Airborne platform Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Develop, integrate and demonstrate a 2-micron pulsed Integrated Path Differential Absorption Lidar (IPDA) instrument CO2 Column Measurement from Airborne platform...

  1. Radioisotope spectrometric method to determine diffusion coefficients in metals and alloys

    International Nuclear Information System (INIS)

    A brief description of the spectrometric installation to study diffusion in metals using #betta#-decay radio-isotopes is presented. Diffusion coefficients of nickel in 70% Co-5% Fe-15% Si-10% B amorphous alloy are determined according to #betta#-radiation absorption in diffusion zone. Plate samples of 10x10 mm size and about 300 μm in thickness are used. Diffusion annealing is conducted during 100 hrs. The calculation of the diffusion coefficients has been carried out by the formula I/I0= esup(μsup(2)Dtau)erfc μ √ Dtau, where I0, I is an initial and a final radiation intensity; μ- an absorption coefficient of 63Ni #betta#-ray in the given material (at calculation μ=1.3x106 m-1 was taken); tau- duration of diffusion annealing; D- diffusion coefficient at the designed temperature. The value of the diffusion coefficient of nickel in 70% Co-5% Fe-15% S-10% B amorphous alloy at the temperature of 200 deg C is turned out to be equal to 4x10-21 m2/s. It should be noted that the self-diffusion coefficient of cobalt in Co-Fe alloy, found by extrapolation from high-temperature region, is equal to 10-35 m2/s, i.e. in 14 orders lower than that of the same basis in amorphous alloy

  2. Early in-flight detection of SO2 via Differential Optical Absorption Spectroscopy: a feasible aviation safety measure to prevent potential encounters with volcanic plumes

    Directory of Open Access Journals (Sweden)

    J. M. Alvarez Nieves

    2011-05-01

    Full Text Available Volcanic ash constitutes a risk to aviation, mainly due to its ability to cause jet engines to fail. Other risks include the possibility of abrasion of windshields and potentially serious damage to avionic systems. These hazards have been widely recognized since the early 1980s, when volcanic ash provoked several incidents of engine failure in commercial aircraft. In addition to volcanic ash, volcanic gases also pose a threat. Prolonged and/or cumulative exposure to sulphur dioxide (SO2 or sulphuric acid (H2SO4 aerosols potentially affects e.g. windows, air frame and may cause permanent damage to engines. SO2 receives most attention among the gas species commonly found in volcanic plumes because its presence above the lower troposphere is a clear proxy for a volcanic cloud and indicates that fine ash could also be present. Up to now, remote sensing of SO2 via Differential Optical Absorption Spectroscopy (DOAS in the ultraviolet spectral region has been used to measure volcanic clouds from ground based, airborne and satellite platforms. Attention has been given to volcanic emission strength, chemistry inside volcanic clouds and measurement procedures were adapted accordingly. Here we present a set of experimental and model results, highlighting the feasibility of DOAS to be used as an airborne early detection system of SO2 in two spatial dimensions. In order to prove our new concept, simultaneous airborne and ground-based measurements of the plume of Popocatépetl volcano, Mexico, were conducted in April 2010. The plume extended at an altitude around 5250 m above sea level and was approached and traversed at the same altitude with several forward looking DOAS systems aboard an airplane. These DOAS systems measured SO2 in the flight direction and at ± 40 mrad (2.3° angles relative to it in both, horizontal and vertical directions. The approaches started at up to 25 km distance to the plume and SO2 was measured at all times well above the

  3. Early in-flight detection of SO2 via Differential Optical Absorption Spectroscopy: a feasible aviation safety measure to prevent potential encounters with volcanic plumes

    Directory of Open Access Journals (Sweden)

    U. Platt

    2011-09-01

    Full Text Available Volcanic ash constitutes a risk to aviation, mainly due to its ability to cause jet engines to fail. Other risks include the possibility of abrasion of windshields and potentially serious damage to avionic systems. These hazards have been widely recognized since the early 1980s, when volcanic ash provoked several incidents of engine failure in commercial aircraft. In addition to volcanic ash, volcanic gases also pose a threat. Prolonged and/or cumulative exposure to sulphur dioxide (SO2 or sulphuric acid (H2SO4 aerosols potentially affects e.g. windows, air frame and may cause permanent damage to engines. SO2 receives most attention among the gas species commonly found in volcanic plumes because its presence above the lower troposphere is a clear proxy for a volcanic cloud and indicates that fine ash could also be present. Up to now, remote sensing of SO2 via Differential Optical Absorption Spectroscopy (DOAS in the ultraviolet spectral region has been used to measure volcanic clouds from ground based, airborne and satellite platforms. Attention has been given to volcanic emission strength, chemistry inside volcanic clouds and measurement procedures were adapted accordingly. Here we present a set of experimental and model results, highlighting the feasibility of DOAS to be used as an airborne early detection system of SO2 in two spatial dimensions. In order to prove our new concept, simultaneous airborne and ground-based measurements of the plume of Popocatépetl volcano, Mexico, were conducted in April 2010. The plume extended at an altitude around 5250 m above sea level and was approached and traversed at the same altitude with several forward looking DOAS systems aboard an airplane. These DOAS systems measured SO2 in the flight direction and at ±40 mrad (2.3° angles relative to it in both, horizontal and vertical directions. The approaches started at up to 25 km distance to the plume and SO2 was measured at all times well above the

  4. Early in-flight detection of SO2 via Differential Optical Absorption Spectroscopy: A feasible aviation safety measure to prevent potential encounters with volcanic plumes

    Science.gov (United States)

    Vogel, L.; Galle, B.; Kern, C.; Delgado, Granados H.; Conde, V.; Norman, P.; Arellano, S.; Landgren, O.; Lubcke, P.; Alvarez, Nieves J.M.; Cardenas, Gonzales L.; Platt, U.

    2011-01-01

    Volcanic ash constitutes a risk to aviation, mainly due to its ability to cause jet engines to fail. Other risks include the possibility of abrasion of windshields and potentially serious damage to avionic systems. These hazards have been widely recognized 5 since the early 1980s, when volcanic ash provoked several incidents of engine failure in commercial aircraft. In addition to volcanic ash, volcanic gases also pose a threat. Prolonged and/or cumulative exposure to sulphur dioxide (SO2) or sulphuric acid (H2SO4) aerosols potentially affects e.g. windows, air frame and may cause permanent damage to engines. SO2 receives most attention among the gas species commonly found in 10 volcanic plumes because its presence above the lower troposphere is a clear proxy for a volcanic cloud and indicates that fine ash could also be present. Up to now, remote sensing of SO2 via Differential Optical Absorption Spectroscopy (DOAS) in the ultraviolet spectral region has been used to measure volcanic clouds from ground based, airborne and satellite platforms. Attention has been given to vol- 15 canic emission strength, chemistry inside volcanic clouds and measurement procedures were adapted accordingly. Here we present a set of experimental and model results, highlighting the feasibility of DOAS to be used as an airborne early detection system of SO2 in two spatial dimensions. In order to prove our new concept, simultaneous airborne and ground-based measurements of the plume of Popocatepetl volcano, Mexico, were conducted in April 2010. The plume extended at an altitude around 5250 m above sea level and was approached and traversed at the same altitude with several forward looking DOAS systems aboard an airplane. These DOAS systems measured SO2 in the flight direction and at ±40 mrad (2.3◦) angles relative to it in both, horizontal and vertical directions. The approaches started at up to 25 km distance to 25 the plume and SO2 was measured at all times well above the detection

  5. Challenges and recent advances in mass spectrometric imaging of neurotransmitters

    OpenAIRE

    Gemperline, Erin; Chen, Bingming; Li, Lingjun

    2014-01-01

    Mass spectrometric imaging (MSI) is a powerful tool that grants the ability to investigate a broad mass range of molecules, from small molecules to large proteins, by creating detailed distribution maps of selected compounds. To date, MSI has demonstrated its versatility in the study of neurotransmitters and neuropeptides of different classes toward investigation of neurobiological functions and diseases. These studies have provided significant insight in neurobiology over the years and curre...

  6. Electrospray Ionization Mass Spectrometric Analysis of Highly Reactive Glycosyl Halides

    Directory of Open Access Journals (Sweden)

    Lajos Kovács

    2012-07-01

    Full Text Available Highly reactive glycosyl chlorides and bromides have been analysed by a routine mass spectrometric method using electrospray ionization and lithium salt adduct-forming agents in anhydrous acetonitrile solution, providing salient lithiated molecular ions [M+Li]+, [2M+Li]+ etc. The role of other adduct-forming salts has also been evaluated. The lithium salt method is useful for accurate mass determination of these highly sensitive compounds.

  7. System for Gamma an X rays fluorescence spectrometric

    International Nuclear Information System (INIS)

    A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

  8. Mass Spectrometric Analysis of Water-soluble Gold Nanoclusters

    International Nuclear Information System (INIS)

    Batches of water-soluble gold nanoclusters of nominal 2.0 or 3.5-nm diameter were prepared to evaluate particle size determinations by a number of techniques such as transmission electron microscopy or atomic force microscopy and to validate estimates derived by mass spectrometric analysis using matrix-assisted laser desorption ionization (MALDI). Good agreement was found and MALDI lends itself to analyses even in the presence of aggregates

  9. Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of some fluoroquinolone antibacterials using ammonium reineckate

    Science.gov (United States)

    Al-Ghannam, Sheikha M.

    2008-04-01

    Three accurate, rapid and simple atomic absorption spectrometric (AAS), conductometric and colorimetric methods were developed for the determination of gatifloxacin (GTF), moxifloxacin (MXF) and sparfloxacin (SPF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at λmax 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone. The optimizations of various experimental conditions were described. Optimum concentration ranges for the determination of GTF, MXF and SPF were 5.0-150, 40-440 μg mL -1 and 0.10-1.5 mg mL -1 using atomic absorption (AAS), conductometric and colorimetric methods, respectively. Detection and quantification limits are ranges from 1.5 to 2.3 μg mL -1 using AAS method or 30-45 μg mL -1 using colorimetric method. The proposed procedures have been applied successfully to the analysis of these drugs in pharmaceutical formulations and the results are favourably comparable to the reference methods.

  10. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  11. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Bentlin, Fabrina R S; Pozebon, Dirce; Mello, Paola A; Flores, Erico M M

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO3)2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 microg g(-1) of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES).

  12. Flame atomic absorption spectrometric determinations of some trace metals after coprecipitation with gold-APDC

    International Nuclear Information System (INIS)

    Complete text of publication follows. For the determination of trace metals in various samples, preconcentration is an inevitable step to overcome interferences. Among various techniques for the separation of trace metals proposed until now, coprecipitation is one of the most useful ones. Many different coprecipitation procedures including use of organic and inorganic collectors have been developed. So far, in the literature, it is reported that APDC, NaDDTC, PAN, TAR, Oxine, etc. as chelating agent for metal-chelate collector have been extensively used for coprecipitation of trace metals. However, metal chelates, especially dithocarbamates, as collectors are ideal for their sensitivities, simplicities and tolerances to interferences.Therefore, in the present work, fundamental studies on the coprecipitation with gold/APDC chelate have been carried out for determination of trace metals in environmental samples by FAAS with microinjection. According to our literature survey, gold/APDC is not used for the coprecipitation of heavy metal ions, until now. In this work, the coprecipitation was carried out in a centrifuge tube. Firstly, the main factors, such as amount of coprecipitant reagent and carrier element, pH of the solution, standing time, sample volume and diverse ions, affecting the coprecipitation of some trace metals were evaluated. Under optimized conditions, the recoveries of Cu, Ni, Pb and Cd were ≥ 95 %. R.S.D. values for ten replicates were lower than 5.0 %. Preconcentration factors were found to be 20. The coprecipitation was applied to various water samples and non-alcoholic beverage.

  13. Evaluation of microwave digestion and solvent extraction for the determination of trace amounts of selenium in feeds and plant and animal tissues by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Hocquellet, P; Candillier, M P

    1991-05-01

    A sensitive method for the accurate determination of Se in agricultural products at sub-ppm levels is described. The proposed procedure involves the wet oxidation of samples by using a mixture of nitric, sulphuric and perchloric acids, co-extraction of Se and added Pd with diethylammonium N,N-diethyldithiocarbamate in chloroform, and electrothermal atomic absorption spectrometric determination of Se in the organic extract. Atomization and extraction conditions are discussed. Special attention is given to the wet oxidation step, and its advantages in speed and simplicity over conventional heating have been evaluated using an automated microwave digestion system. The results reported, obtained from several reference materials, confirm the accuracy of the method with which a detection limit of 0.002 micrograms g-1 of Se can be achieved. PMID:1877754

  14. Application of cloud point preconcentration and flame atomic absorption spectrometry for the determination of cadmium and zinc ions in urine, blood serum and water samples

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2013-01-01

    Full Text Available A simple, sensitive and selective cloud point extraction procedure is described for the preconcentration and atomic absorption spectrometric determination of Zn2+ and Cd2+ ions in water and biological samples, after complexation with 3,3',3",3'"-tetraindolyl (terephthaloyl dimethane (TTDM in basic medium, using Triton X-114 as nonionic surfactant. Detection limits of 3.0 and 2.0 µg L-1 and quantification limits 10.0 and 7.0 µg L-1were obtained for Zn2+ and Cd2+ ions, respectively. Relative standard deviation was 2.9 and 3.3, and enrichment factors 23.9 and 25.6, for Zn2+ and Cd2+ ions, respectively. The method enabled determination of low levels of Zn2+ and Cd2+ ions in urine, blood serum and water samples.

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

    Energy Technology Data Exchange (ETDEWEB)

    Foss, G. O.

    1981-10-01

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

  16. Mass Spectrometric Calibration of Controlled Fluoroform Leak Rate Devices Technique and Uncertainty Analysis

    CERN Document Server

    Balsley, S D; Laduca, C A

    2003-01-01

    Controlled leak rate devices of fluoroform on the order of 10 sup - sup 8 atm centre dot cc sec sup - sup 1 at 25 C are used to calibrate QC-1 War Reserve neutron tube exhaust stations for leak detection sensitivity. Close-out calibration of these tritium-contaminated devices is provided by the Gas Dynamics and Mass Spectrometry Laboratory, Organization 14406, which is a tritium analytical facility. The mass spectrometric technique used for the measurement is discussed, as is the first principals calculation (pressure, volume, temperature and time). The uncertainty of the measurement is largely driven by contributing factors in the determination of P, V and T. The expanded uncertainty of the leak rate measurement is shown to be 4.42%, with a coverage factor of 3 (k=3).

  17. Mass spectrometric imaging of flavonoid glycosides and biflavonoids in Ginkgo biloba L.

    Science.gov (United States)

    Beck, Sebastian; Stengel, Julia

    2016-10-01

    Ginkgo biloba L. is known to be rich in flavonoids and flavonoid glycosides. However, the distribution within specific plant organs (e.g. within leaves) is not known. By using HPLC-MS and MS/MS we have identified a number of previously known G. biloba flavonoid glycosides and biflavonoids from leaves. Namely, kaempferol, quercetin, isorhamnetin, myricetin, laricitrin/mearnsetin and apigenin glycosides were identified. Furthermore, biflavonoids like ginkgetin/isoginkgetin were also detected. The application of MALDI mass spectrometric imaging, enabled the compilation of concentration profiles of flavonoid glycosides and biflavonoids in G. biloba L. leaves. Both, flavonoid glycosides and biflavonoids show a distinct distribution in leaf thin sections of G. biloba L. PMID:27233155

  18. Simple hollow fiber renewal liquid membrane extraction method for pre-concentration of Cd(II) in environmental samples and detection by Flame Atomic Absorption Spectrometry

    International Nuclear Information System (INIS)

    A hollow fiber renewal liquid membrane (HFRLM) extraction method to determine cadmium (II) in water samples using Flame Atomic Absorption Spectrometry (FAAS) was developed. Ammonium O,O-diethyl dithiophosphate (DDTP) was used to complex cadmium (II) in an acid medium to obtain a neutral hydrophobic complex (ML2). The organic solvent introduced to the sample extracts this complex from the aqueous solution and carries it over the poly(dimethylsiloxane) (PDMS) membrane, that had their walls previously filled with the same organic solvent. The organic solvent is solubilized inside the PDMS membrane, leading to a homogeneous phase. The complex strips the lumen of the membrane where, at higher pH, the complex Cd-DDTP is broken down and cadmium (II) is released into the stripping phase. EDTA was used to complex the cadmium (II), helping to trap the analyte in the stripping phase. A multivariate procedure was used to optimize the studied variables. The optimized variables were: sample (donor phase) pH 3.25, DDTP concentration 0.05% (m/v), stripping (acceptor phase) pH 8.75, EDTA concentration 1.5 x 10-2 mol L-1, extraction temperature 40 deg. C, extraction time 40 min, a solvent mixture N-butyl acetate and hexane (60/40%, v/v) with a volume of 100 μL, and addition of ammonium sulfate to saturate the sample. The sample volume used was 20 mL and the stripping volume was 165 μL. The analyte enrichment factor was 120, limit of detection (LOD) 1.3 μg L-1, relative standard deviation (RSD) 5.5% and the working linear range 2-30 μg L-1.

  19. V oxidation state in Fe-Ti oxides by high-energy resolution fluorescence-detected X-ray absorption spectroscopy

    Science.gov (United States)

    Bordage, Amélie; Balan, Etienne; de Villiers, Johan P. R.; Cromarty, Robert; Juhin, Amélie; Carvallo, Claire; Calas, Georges; Sunder Raju, P. V.; Glatzel, Pieter

    2011-06-01

    The oxidation state of vanadium in natural and synthetic Fe-Ti oxides is determined using high-energy resolution fluorescence-detected X-ray absorption spectroscopy (HERFD-XAS). Eleven natural magnetite-bearing samples from a borehole of the Main Magnetite Layer of the Bushveld Complex (South Africa), five synthetic Fe oxide samples, and three natural hematite-bearing samples from Dharwar supergroup (India) are investigated. V K edge spectra were recorded on the ID26 beamline at the European Synchrotron Radiation Facility (Grenoble, France), and the pre-edge features were used to determine the local environment and oxidation state of vanadium. In the case of the magnetite samples (natural and synthetic), we show that vanadium is incorporated in the octahedral site of the spinel structure under two oxidation states: +III and +IV. The variations of the pre-edge area are interpreted as various proportions in V3+ and V4+ (between 9.5 and 16.3% of V4+), V3+ being the main oxidation state. In particular, the variations of the V4+/V3+ ratio along the profile of the Main Magnetite Layer seem to follow the crystallization sequence of the layer. In the case of the hematite samples from India, the pre-edge features indicate that vanadium is substituted to Fe and mainly incorporated as V4+ (between 40 and 72% of V4+). We also demonstrate the potentiality of HERFD-XAS for mineralogical studies, since it can filter out the unwanted fluorescence and give better resolved spectra than conventional XAS.

  20. Metallomics approach to trace element analysis in ustilago maydis using cellular fractionation, atomic absorption spectrometry, and size exclusion chromatography with ICP-MS detection.

    Science.gov (United States)

    Muñoz, Alma Hortensia Serafin; Kubachka, Kevin; Wrobel, Kazimierz; Corona, Felix Gutierrez; Yathavakilla, Santha K V; Caruso, Joseph A; Wrobel, Katarzyna

    2005-06-29

    Huitlacoche is the ethnic name of the young fruiting bodies of Ustilago maydis, a common parasite of maize. In Mexico and other Latin American countries, this fungus has been traditionally appreciated as a local delicacy. In this work a metallomics approach was used with the determination of eight elements in huitlacoche by electrothermal atomic absorption spectrometry as one facet of this approach. The results obtained indicated relatively lower concentrations of commonly analyzed metals, as referred to the data reported for other mushroom types. This effect was ascribed to different accessibilities of elements, depending on fungus substrate (lower from plant than from soil). Subcellular fractionation was accomplished by centrifugation of cell homogenates suspended in Tris-HCl buffer. Recoveries of the fractionation procedure were in the range of 71-103%. For six elements (Cr, Cu, Fe, Mn, Ni, and Pb), the mean relative contributions in cytosol, cell walls, and mixed membrane fraction were 50.7, 48.2, and 1.1% respectively. To attain the molecular weight distribution of compounds containing target elements as an additional aspect of the metallomics approach, the fungus extract (1% sodium dodecyl sulfate in Tris-HCl, 30 mmol L(-)(1), pH 7.0) was analyzed by size exclusion chromatography with UV and ICP-MS detection. With spectrophotometric detection (280 nm), the elution of high molecular weight compounds was observed in the form of one peak (MW > 10 kDa), and several lower peaks appeared at higher retention times (MW < 10 kDa). On ICP-MS chromatograms, a coelution of (59)Co, (63)Cu, (57)Fe, (202)Hg, (60)Ni, and (80)Se with the first peak on the UV chromatogram was clearly observed, indicating that a fraction of each element incorporated with high molecular weight compounds (12.7, 19.8, 33.7, 100, 19.4, and 45.8%, respectively, based on the peak area measurements). From a comparison of (80)Se and (33)S chromatograms (for sulfur analysis, the extract was obtained in

  1. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Young Wook; Nam, Dae Young; Kang, Kyoung Hoon; Ha, Kyung Wook; Han, In Hee; Chang, Byung Kon; Yoon, Mi Kyeong; Lee, Jae Hwi [Chung-Ang University, Seoul (Korea, Republic of)

    2006-02-15

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C{sub 18} column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

  2. Mass spectrometric analysis of laser evaporation products of ceramics of Bi2Sr2CaCu2Ox composition

    International Nuclear Information System (INIS)

    Mass spectrometric analysis is used to study mechanism of laser evaporation of superconducting ceramics of Bi2Sr2CaCu2Ox composition. During evaporation as a result of pulsed laser irradiation of a sample placed in vaccum ions of all metals containing in ceramics and also neutral O2, Ca, Sr, Cu, Bi and metal oxides were detected on yttrium aluminate. Time-of-flight spectra had two peaks corresponding to ion and neutral components. Comparison of neutral components. Comparison of neutral particle rates points to the fact that gas dynamic processes connected with formation of dense gas cloud near the target surface play an important

  3. MgII Absorption Lines in z=2.974 Damped Lyman-alpha System toward Gravitationally Lensed QSO APM 08279+5255 Detection of Small-scale Structure in MgII Absorbing Clouds

    CERN Document Server

    Kobayashi, N; Goto, M; Tokunaga, A; Kobayashi, Naoto; Terada, Hiroshi; Goto, Miwa; Tokunaga, Alan

    2002-01-01

    1.02-1.16 micron spectra (R ~ 7,000) of the gravitationally lensed QSO APM 08279+5255 at z_em=3.911 were obtained during the commissioning run of IRCS, the 1-5 micron near-infrared camera and spectrograph for the Subaru 8.2 m Telescope. Strong MgII doublet at 2976,2800 angstrom and FeII (2600 angstrom), FeII (2587 angstrom) absorption lines at z_abs=2.974 were clearly detected in the rest-frame UV spectra, confirming the presence of a damped Lyman-alpha system at the redshift as suggested by Petitjean et al. Also MgI (2853 angstrom) absorption line is probably detected. An analysis of the absorption lines including velocity decomposition was performed. This is a first detailed study of MgII absorption system at high redshift (z > 2.5) where the MgII doublet shifts into the near-infrared in the observer's frame. The spectra of the lensed QSO pair A and B with 0.38 arcsec separation were resolved in some exposure frames under excellent seeing condition. We extracted the MgII doublet spectra of A and B separatel...

  4. Mass Spectrometric Analysis of Histone Proteoforms

    Science.gov (United States)

    Yuan, Zuo-Fei; Arnaudo, Anna M.; Garcia, Benjamin A.

    2014-06-01

    Histones play important roles in chromatin, in the forms of various posttranslational modifications (PTMs) and sequence variants, which are called histone proteoforms. Investigating modifications and variants is an ongoing challenge. Previous methods are based on antibodies, and because they usually detect only one modification at a time, they are not suitable for studying the various combinations of modifications on histones. Fortunately, mass spectrometry (MS) has emerged as a high-throughput technology for histone analysis and does not require prior knowledge about any modifications. From the data generated by mass spectrometers, both identification and quantification of modifications, as well as variants, can be obtained easily. On the basis of this information, the functions of histones in various cellular contexts can be revealed. Therefore, MS continues to play an important role in the study of histone proteoforms. In this review, we discuss the analysis strategies of MS, their applications on histones, and some key remaining challenges.

  5. The HI absorption 'Zoo'

    CERN Document Server

    Gereb, K; Morganti, R; Oosterloo, T A

    2014-01-01

    We present an analysis of the HI absorption in a sample of 101 flux-selected radio AGN (S_1.4 GHz > 50 mJy) observed with the Westerbork Synthesis Radio Telescope (WSRT). HI absorption is detected in 32 galaxies, showing a broad variety of widths, shapes and kinematical properties. We characterize the HI spectra of the individual detections using the busy function (Westmeier et al. 2014). With the goal of identifying different morphological structures of HI, we study the kinematical and radio source properties of the detections as function of their width. Narrow lines (FWHM = 500 km/s). These detections are good candidates for being HI outflows. The detection rate of HI outflows is 5 percent in the total radio AGN sample. This fraction represents a lower limit, however it could suggests that, if outflows are a characteristic phenomenon of all radio sources, they would have a short depletion timescale compared to the lifetime of the AGN. Blueshifted and broad/asymmetric lines are more often present among young...

  6. FITPix COMBO—Timepix detector with integrated analog signal spectrometric readout

    Science.gov (United States)

    Holik, M.; Kraus, V.; Georgiev, V.; Granja, C.

    2016-02-01

    The hybrid semiconductor pixel detector Timepix has proven a powerful tool in radiation detection and imaging. Energy loss and directional sensitivity as well as particle type resolving power are possible by high resolution particle tracking and per-pixel energy and quantum-counting capability. The spectrometric resolving power of the detector can be further enhanced by analyzing the analog signal of the detector common sensor electrode (also called back-side pulse). In this work we present a new compact readout interface, based on the FITPix readout architecture, extended with integrated analog electronics for the detector's common sensor signal. Integrating simultaneous operation of the digital per-pixel information with the common sensor (called also back-side electrode) analog pulse processing circuitry into one device enhances the detector capabilities and opens new applications. Thanks to noise suppression and built-in electromagnetic interference shielding the common hardware platform enables parallel analog signal spectroscopy on the back side pulse signal with full operation and read-out of the pixelated digital part, the noise level is 600 keV and spectrometric resolution around 100 keV for 5.5 MeV alpha particles. Self-triggering is implemented with delay of few tens of ns making use of adjustable low-energy threshold of the particle analog signal amplitude. The digital pixelated full frame can be thus triggered and recorded together with the common sensor analog signal. The waveform, which is sampled with frequency 100 MHz, can be recorded in adjustable time window including time prior to the trigger level. An integrated software tool provides control, on-line display and read-out of both analog and digital channels. Both the pixelated digital record and the analog waveform are synchronized and written out by common time stamp.

  7. The hydrolysis of aluminium, a mass spectrometric study

    OpenAIRE

    Sarpola, A.

    2007-01-01

    Abstract This thesis is focused on the hydrolysis of aluminium, the polymerisation of the hydrolysis products, and how these can be monitored by mass spectrometric methods. The main aim of this research is to figure out how the aqueous speciation of aluminium changes as a function of pH (3.2–10), concentration (1–100 mM), reaction time (1s–14d), and counter anion (Cl-, SO42-, HCOO-). The method used was electrospray mass spectrometry. The results showed more variable speciation than those ...

  8. Visualization of High Resolution Spatial Mass Spectrometric Data during Acquisition

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, Mathew; Heath, Brandi S.; Laskin, Julia; Li, Dongsheng; Liu, Ellen C.; Hui, Katrina L.; Kuprat, Andrew P.; Kleese van Dam, Kerstin; Carson, James P.

    2012-08-28

    Mass Spectrometric Imaging (IMS) allows the generation of 2D ion density maps that help visualize molecules present in sections of tissues and cells. The combination of spatial and mass resolution results in large and complex data sets that require powerful and efficient analysis and interpretation. In this paper, a graphical user interface (GUI) that can visualize the large data during data acquisition itself is presented. The program also has the ability to perform processing and analysis of the dataset. The various functions of the GUI including visualization of mass spectra, generation of 2D maps for selected species, manipulation of the heat maps, and peak identification are also presented.

  9. Mass spectrometric imaging of ginsenosides localization in Panax ginseng root

    OpenAIRE

    Taira, Shu; Ikeda, Ryuzo; Yokota, Naohiko; OSAKA, Issey; Sakamoto, Manabu; Kato, Mitsuro; Sahashi, Yuko

    2010-01-01

    We succeeded in performing mass spectrometric imaging (MSI) of the localization of ginsenosides (Rb_1, Rb_2 or R_c, and Rf) in cross-sections of the Panax ginseng root at a resolution of 100 μm using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Tandem mass spectrometry (MS/MS) of alkali metal-adducted ginsenoside ions revealed structural information of the corresponding saccharides and agricones. MALDI-MSI confirmed that localization of ginsenosides in the cortex ...

  10. Ultratrace determination of tin by hydride generation in-atomizer trapping atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Průša, Libor [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Charles University in Prague, Faculty of Science, Department of Analytical Chemistry, Hlavova 8, Prague 2, CZ 128 43 Czech Republic (Czech Republic); Dědina, Jiří [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Kratzer, Jan, E-mail: jkratzer@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2013-12-04

    Graphical abstract: -- Highlights: •In-atomizer trapping HG-AAS was optimized for Sn. •A compact quartz trap-and-atomizer device was employed. •Generation, preconcentration and atomization steps were investigated in detail. •Hundred percent preconcentration efficiency for tin was reached. •Routine analytical method was developed for Sn determination (LOD of 0.03 ng mL{sup −1} Sn). -- Abstract: A quartz multiatomizer with its inlet arm modified to serve as a trap (trap-and-atomizer device) was employed to trap tin hydride and subsequently to volatilize collected analyte species with atomic absorption spectrometric detection. Generation, atomization and preconcentration conditions were optimized and analytical figures of merit of both on-line atomization as well as preconcentration modes were quantified. Preconcentration efficiency of 95 ± 5% was found. The detection limits reached were 0.029 and 0.14 ng mL{sup −1} Sn, respectively, for 120 s preconcentration period and on-line atomization mode without any preconcentration. The interference extent of other hydride forming elements (As, Se, Sb and Bi) on tin determination was found negligible in both modes of operation. The applicability of the developed preconcentration method was verified by Sn determination in a certified reference material as well as by analysis of real samples.

  11. Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.;

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...

  12. Separation of seven arsenic compounds by high-performance liquid chromatography with on-line detection by hydrogen–argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, S. H.; Larsen, E. H.; Pritzl, G.;

    1992-01-01

    Seven molecular forms of arsenic were separated by anion- and cation-exchange high-performance liquid chromatography (HPLC) with on-line detection by flame atomic absorption spectrometry (FAAS). The interfacing was established by a vented poly(tetrafluoroethylene) capillary tubing connecting......-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...

  13. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    Energy Technology Data Exchange (ETDEWEB)

    1981-01-01

    Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, impurity content. The following analytical procedures, which are described in detail, are designed to show whether or not a given material meets specifications: uranium by ferrous sulfate reduction in phosphoric acid and dichromate titration method; uranium and oxygen uranium atomic ratio by the ignition (gravimetric) impurity correction method; oxygen to uranium atomic ratios by the polarographic method; carbon (total) by direct combustion-thermal conductivity method; total chlorine and fluorine by pyrohydrolysis ion-selective electrode method; moisture by the coulometric, electrolytic moisture analyzer method; nitrogen by the Kjeldahl method; total sulfur by distillation-spectrophotometric method; isotopic uranium composition by multiple-filament surface-ionization mass spectrometric method; spectrochemical determination of trace elements in high-purity uranium dioxide; volatile fluoride impurities by spectrochemical method using the rotating-disk spark technique; spectrochemical determination of silver by gallium oxide carrier D-C arc technique; rare earths by copper spark-spectrochemical method; impurity elements by a spark-source mass spectrographic method; surface area by nitrogen absorption method; total gas in reactor-grade uranium dioxide pellets; thorium and rare earth elements by spectroscopy; hydrogen by inert gas fusion; and uranium isotopic analysis by mass spectrometry. (JMT)

  14. Acoustic absorption by sunspots

    Science.gov (United States)

    Braun, D. C.; Labonte, B. J.; Duvall, T. L., Jr.

    1987-01-01

    The paper presents the initial results of a series of observations designed to probe the nature of sunspots by detecting their influence on high-degree p-mode oscillations in the surrounding photosphere. The analysis decomposes the observed oscillations into radially propagating waves described by Hankel functions in a cylindrical coordinate system centered on the sunspot. From measurements of the differences in power between waves traveling outward and inward, it is demonstrated that sunspots appear to absorb as much as 50 percent of the incoming acoustic waves. It is found that for all three sunspots observed, the amount of absorption increases linearly with horizontal wavenumber. The effect is present in p-mode oscillations with wavelengths both significantly larger and smaller than the diameter of the sunspot umbrae. Actual absorption of acoustic energy of the magnitude observed may produce measurable decreases in the power and lifetimes of high-degree p-mode oscillations during periods of high solar activity.

  15. Acoustic absorption by sunspots

    Energy Technology Data Exchange (ETDEWEB)

    Braun, D.C.; Labonte, B.J.; Duvall, T.L. Jr.

    1987-08-01

    The paper presents the initial results of a series of observations designed to probe the nature of sunspots by detecting their influence on high-degree p-mode oscillations in the surrounding photosphere. The analysis decomposes the observed oscillations into radially propagating waves described by Hankel functions in a cylindrical coordinate system centered on the sunspot. From measurements of the differences in power between waves traveling outward and inward, it is demonstrated that sunspots appear to absorb as much as 50 percent of the incoming acoustic waves. It is found that for all three sunspots observed, the amount of absorption increases linearly with horizontal wavenumber. The effect is present in p-mode oscillations with wavelengths both significantly larger and smaller than the diameter of the sunspot umbrae. Actual absorption of acoustic energy of the magnitude observed may produce measurable decreases in the power and lifetimes of high-degree p-mode oscillations during periods of high solar activity. 10 references.

  16. Column system using diaion HP-2MG for determination of some metal ions by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa; Soylak, Mustafa

    2004-02-23

    A column solid-phase extraction method for the preconcentration and determination of cadmium(II), copper(II), cobalt(II), iron(III), lead(II), nickel(II) and zinc(II) dithizone chelates by atomic absorption spectrometry has been described. Diaion HP-2MG was used as adsorbent for column studies. The influences of the various analytical parameters including pH of the aqueous solutions, amounts of ligand and resin were investigated for the retentions of the analyte ions. The recovery values are ranged from 95 to 102%. The influences of alkaline and earth alkaline ions were also discussed. The preconcentration factor was 375, when the sample volume and final volume are 750 and 2 ml, respectively. The detection limits of the analyte ions (k=3, N=21) were varying 0.08 {mu}g/l for cadmium to 0.25 {mu}g/l for lead. The relative standard deviations of the determinations at the concentration range of 1.8x10{sup -4} to 4.5x10{sup -5} mmol for the investigated elements were found to be lower than 9%. The proposed solid-phase extraction procedure were applied to the flame atomic absorption spectrometric determinations of analyte ions in natural waters (sea, tap, river), microwave digested samples (milk, red wine and rice) and two different reference standard materials (SRM1515 apple leaves and NRCC-SLRS-4 riverine water)

  17. Study on detection of pesticide residue based on spectroscopy technology of differential absorption%基子光谱差分吸收技术的农药残留检测研究

    Institute of Scientific and Technical Information of China (English)

    赵明富; 胡建敢; 全晓莉; 刘杰徽; 曹雪梅

    2012-01-01

    For the domestic food safety problem that caused by the pesticide residues in food,it's very important that research a convenient and cost-appropriate detection technology.At present,spectroscopy absorption technology has been used for detection of pesticide residues in food.However,there are some deficiencies such as the quantitative detection and the measurement precision.This experiment that based on differential absorption is completed by using miniature fiber optic spectrometer and spectrophotometer,and then the pesticide dichlorvos is also measured quantitatively.Thus the pesticide residue detection technology that based on spectroscopy absorption is improved to adjust to the practical application.%针对国内主要食品中广泛存在的农药残留带来的食品安全问题,研究一种方便快捷且成本适宜的检测技术,具有重要的意义。目前,已有相关实验将光谱吸收技术用于食品农药残留检测,但是,对于定量检测及测量精度方面该实验还存在一些不足。本文基于差分吸收技术,采用荷兰Avantes公司的微型光纤光谱仪以及分光光度计,进行了相关实验,实现了对敌敌畏水剂农药的定量测量,从而对基于光谱吸收技术的农药残留检测技术进行了完善,使其更加适合实际应用。

  18. FIRST ULTRAVIOLET REFLECTANCE SPECTRA OF PLUTO AND CHARON BY THE HUBBLE SPACE TELESCOPE COSMIC ORIGINS SPECTROGRAPH: DETECTION OF ABSORPTION FEATURES AND EVIDENCE FOR TEMPORAL CHANGE

    International Nuclear Information System (INIS)

    We have observed the mid-UV spectra of both Pluto and its large satellite, Charon, at two rotational epochs using the Hubble Space Telescope (HST) Cosmic Origins Spectrograph (COS) in 2010. These are the first HST/COS measurements of Pluto and Charon. Here we describe the observations and our reduction of them, and present the albedo spectra, average mid-UV albedos, and albedo slopes we derive from these data. These data reveal evidence for a strong absorption feature in the mid-UV spectrum of Pluto; evidence for temporal change in Pluto's spectrum since the 1990s is reported, and indirect evidence for a near-UV spectral absorption on Charon is also reported.

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

    Energy Technology Data Exchange (ETDEWEB)

    Gil, Raúl A.; Pacheco, Pablo H.; Cerutti, Soledad [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Martinez, Luis D., E-mail: ldm@unsl.edu.ar [Área de Química Analítica, Facultad de Química Bioquímica y Farmacia, Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina); Instituto de Química de San Luis, INQUISAL, Centro Científico-Tecnológico de San Luis (CCT-San Luis), Consejo Nacional de Investigaciones Científicas y Universidad Nacional de San Luis, Ciudad de San Luis 5700 (Argentina)

    2015-05-22

    This article reviews 120 articles found in SCOPUS and specific Journal cites corresponding to the terms ‘preconcentration’; ‘speciation’; ‘vapor generation techniques’ and ‘atomic spectrometry techniques’ in the last 5 years. - Highlights: • Recent advances in vapor generation and atomic spectrometry were reviewed. • Species-specific preconcentration strategies after and before VG were discussed. • New preconcentration and speciation analysis were evaluated within this framework. - Abstract: We review recent progress in preconcentration strategies associated to vapor generation techniques coupled to atomic spectrometric (VGT-AS) for specific chemical species detection. This discussion focuses on the central role of different preconcentration approaches, both before and after VG process. The former was based on the classical solid phase and liquid–liquid extraction procedures which, aided by automation and miniaturization strategies, have strengthened the role of VGT-AS in several research fields including environmental, clinical, and others. We then examine some of the new vapor trapping strategies (atom-trapping, hydride trapping, cryotrapping) that entail improvements in selectivity through interference elimination, but also they allow reaching ultra-low detection limits for a large number of chemical species generated in conventional VG systems, including complete separation of several species of the same element. This review covers more than 100 bibliographic references from 2009 up to date, found in SCOPUS database and in individual searches in specific journals. We finally conclude by giving some outlook on future directions of this field.

  20. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Energy Technology Data Exchange (ETDEWEB)

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  1. Advances in Mass Spectrometric Tools for Probing Neuropeptides

    Science.gov (United States)

    Buchberger, Amanda; Yu, Qing; Li, Lingjun

    2015-07-01

    Neuropeptides are important mediators in the functionality of the brain and other neurological organs. Because neuropeptides exist in a wide range of concentrations, appropriate characterization methods are needed to provide dynamic, chemical, and spatial information. Mass spectrometry and compatible tools have been a popular choice in analyzing neuropeptides. There have been several advances and challenges, both of which are the focus of this review. Discussions range from sample collection to bioinformatic tools, although avenues such as quantitation and imaging are included. Further development of the presented methods for neuropeptidomic mass spectrometric analysis is inevitable, which will lead to a further understanding of the complex interplay of neuropeptides and other signaling molecules in the nervous system.

  2. Vitamin D-metabolites from human plasma and mass spectrometric analysis by fast heavy ion induced desorption

    International Nuclear Information System (INIS)

    D-vitamin metabolites have been isolated from human serum employing chromatographic techniques. The serum carrier protein for vitamin D (DBP) was first isolated by immunosorbent chromatography. Lipid ligands associated with DBP were then extracted with hexane and separated by high pressure liquid chromatography (HPLC). Detection of vitamin D metabolites by their absorbance of ultraviolet light is not sufficiently sensitive to monitor all vitamin D derivatives from a few millilitres of serum. Therefore, further analyses are necessary to quantitative these compounds. We have begun to develop a mass spectrometric method to achieve a reliable, quantitative procedure. As a first step towards this goal a number of pure samples of vitamin D compounds have been studied in a time-of-flight mass spectrometer based on fast heavy ion induced desorption. All vitamin D compounds examined could be detected and identified by their molecular ion and fragment spectra. (orig.)

  3. Mass spectrometric profiling of flavonoid glycoconjugates possessing isomeric aglycones.

    Science.gov (United States)

    Abrankó, László; Szilvássy, Blanka

    2015-01-01

    In fields such as food and nutrition science or plant physiology, interest in untargeted profiling of flavonoids continues to expand. The group of flavonoids encompasses several thousands of chemically distinguishable compounds, among which are a number of isobaric compounds with the same elemental composition. Thus, the mass spectrometric identification of these compounds is challenging, especially when reference standards are not available to support their identification. Many different types of isomers of flavonoid glycoconjugates are known, i.e. compounds that differ in their glycosylation position, glycan sequence or type of interglycosidic linkage. This work focuses on the mass spectrometric identification of flavonoid glycoconjugate isomers possessing the same glycan mass and differing only in their aglycone core. A non-targeted HPLC-ESI-MS/MS profiling method using a triple quadrupole MS is presented herein, which utilizes in-source fragmentation and a pseudo-MS(3) approach for the selective analysis of flavonoid glycoconjugates with isomeric/isobaric aglycones. A selective MRM-based identification of the in-source formed isobaric aglycone fragments was established. Additionally, utilizing the precursor scanning capability of the employed triple quadrupole instrument, the developed method enabled the determination of the molecular weight of the studied intact flavonoid glycoconjugate. The versatility of the method was proven with various types of flavonoid aglycones, i.e. anthocyanins, flavonols, flavones, flavanones and isoflavones, along with their representative glycoconjugates. The developed method was also successfully applied to a commercially available sour cherry sample, in which 16 different glycoconjugates of pelargonidin, genistein, cyanidin, kaempferol and quercetin could be tentatively identified, including a number of compounds containing isomeric/isobaric aglycones. PMID:25601677

  4. Detection of impaired intestinal absorption of long-chain fatty acids : validation studies of a novel test in a rat model of fat malabsorption

    NARCIS (Netherlands)

    Kalivianakis, M; Minich, DM; Havinga, R; Kuipers, F; Stellaard, F; Vonk, RJ; Verkade, HJ

    2000-01-01

    Background: Classic fat balance studies detect fat malabsorption but do not discriminate between the potential causes of malabsorption, such as impaired intestinal lipolysis or reduced uptake of fatty acids. Objective: We aimed to validate a novel test for the specific, sensitive detection of impair

  5. The HI absorption "Zoo"

    Science.gov (United States)

    Geréb, K.; Maccagni, F. M.; Morganti, R.; Oosterloo, T. A.

    2015-03-01

    We present an analysis of the H I 21 cm absorption in a sample of 101 flux-selected radio AGN (S1.4 GHz> 50 mJy) observed with the Westerbork Synthesis Radio Telescope (WSRT). We detect H I absorption in 32 objects (30% of the sample). In a previous paper, we performed a spectral stacking analysis on the radio sources, while here we characterize the absorption spectra of the individual detections using the recently presented busy function. The H I absorption spectra show a broad variety of widths, shapes, and kinematical properties. The full width half maximum (FWHM) of the busy function fits of the detected H I lines lies in the range 32 km s-1 200 km s-1). We study the kinematical and radio source properties of each group, with the goal of identifying different morphological structures of H I. Narrow lines mostly lie at the systemic velocity and are likely produced by regularly rotating H I disks or gas clouds. More H I disks can be present among galaxies with lines of intermediate widths; however, the H I in these sources is more unsettled. We study the asymmetry parameter and blueshift/redshift distribution of the lines as a function of their width. We find a trend for which narrow profiles are also symmetric, while broad lines are the most asymmetric. Among the broadest lines, more lines appear blueshifted than redshifted, similarly to what was found by previous studies. Interestingly, symmetric broad lines are absent from the sample. We argue that if a profile is broad, it is also asymmetric and shifted relative to the systemic velocity because it is tracing unsettled H I gas. In particular, besides three of the broadest (up to FW20 = 825 km s-1) detections, which are associated with gas-rich mergers, we find three new cases of profiles with blueshifted broad wings (with FW20 ≳ 500 km s-1) in high radio power AGN. These detections are good candidates for being HI outflows. Together with the known cases of outflows already included in the sample (3C 293 and

  6. Method of double tracer addition for determining uranium in geological samples by mass spectrometric isotope dilution

    International Nuclear Information System (INIS)

    The present work shows the experimental details on the uranium determination in materials by mass spectrometric isotope dilution technique with double tracer (233U + 235U). The mass discrimination phenomenon effect is studied. The uranium concentration values obtained by mass spectrometric isotope dilution technique with double tracer are compared with other techniques. The influence of the sampling in the accurate determination of uranium in the rock sample is discussed. (author)

  7. Review of procedures involving separation and preconcentration for the determination of cadmium using spectrometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Sergio L.C. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil)]. E-mail: slcf@ufba.br; Andrade, Jailson B. de [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Korn, Maria das Gracas A. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Pereira, Madson de G. [Departamento de Ciencias Exatas e da Terra Campus 1-Cabula, Universidade do Estado da Bahia, Salvador, Bahia 41195-001 (Brazil); Lemos, Valfredo A. [Laboratorio de Quimica Analitica, Campus de Jequie, Universidade Estadual do Sudoeste da Bahia, Jequie, Bahia 45200-190 (Brazil); Santos, Walter N.L. dos [Departamento de Ciencias Exatas e da Terra Campus 1-Cabula, Universidade do Estado da Bahia, Salvador, Bahia 41195-001 (Brazil); Rodrigues, Frederico de Medeiros [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Empresa Baiana de Desenvolvimento Agricola S.A., Avenida Dorival Caymmi 15649, Itapoan, Salvador, Bahia 41635-150 (Brazil); Souza, Anderson S. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Instituto Multidisciplinar em Saude, Campus AnisioTeixeira, Universidade Federal da Bahia, Vitoria da Conquista, Bahia 45055-090 (Brazil); Ferreira, Hadla S. [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil); Silva, Erik G.P. da [Instituto de Quimica, Campus Universitario Ondina, Universidade Federal da Bahia, Salvador, Bahia 40170-290 (Brazil)

    2007-07-16

    Spectrometric techniques for the analysis of trace cadmium have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, such as electrochemical deposition, precipitation, coprecipitation, solid phase extraction, liquid-liquid extraction (LLE) and cloud point extraction (CPE), and consider the features of the their application with several spectrometric techniques.

  8. Quantum-state resolved reaction dynamics at the gas-liquid interface: Direct absorption detection of HF(v,J) product from F(2P)+squalane

    Science.gov (United States)

    Zolot, Alexander M.; Harper, Warren W.; Perkins, Bradford G.; Dagdigian, Paul J.; Nesbitt, David J.

    2006-07-01

    Exothermic reactive scattering of F atoms at the gas-liquid interface of a liquid hydrocarbon (squalane) surface has been studied under single collision conditions by shot noise limited high-resolution infrared absorption on the nascent HF (v,J) product. The nascent HF (v,J) vibrational distributions are inverted, indicating insufficient time for complete vibrational energy transfer into the surface liquid. The HF (v=2,J) rotational distributions are well fit with a two temperature Boltzmann analysis, with a near room temperature component (TTD≈290K) and a second much hotter scattering component (THDS≈1040K). These data provide quantum state level support for microscopic branching in the atom abstraction dynamics corresponding to escape of nascent HF from the liquid surface on time scales both slow and fast with respect to rotational relaxation.

  9. Mass spectrometric protein characterization in proteome analysis using GELoader tip micro-columns packed with various chromatographic material

    International Nuclear Information System (INIS)

    In the early 90'ies mass spectrometry (MS) was introduced as a tool for identifying proteins in protein sequence databases. Since then it has become an integrated tool in protein characterization and is today routinely used to identify proteins separated by gel electrophoresis. A two-tiered mass spectrometric protein identification strategy has recently been proposed. In the first strategy peptide mass maps obtained from the protein of interest are compared with theoretically derived peptide mass maps from proteins in protein sequence databases. If the protein cannot be identified by this strategy, tandem mass spectrometric sequencing is used to generate enough sequence data to identify the protein in protein sequence databases or expressed sequence tag (EST) databases. However, the above strategies primarily identify a protein relatively to the DNA sequence, in which no information about e.g. post-translational modifications (PTMs) is stored. PTMs are known to modify the function, location, solubility and activity of proteins in the cell, and they are therefore very important for understanding living cells. More than 200 different PTMs are known, of which glycosylation, phosphorylation and proteolytic processing are the most common ones. Mass spectrometric analysis of PTMs on gel-separated proteins requires a higher amount of protein than for identification only. In addition, higher sequence coverage from the peptide mass maps or pre-purification of the modified peptides prior to MS analysis, is necessary for detection of putative modified peptides. In this study a multi-tiered strategy, in which GELoader tip micro-columns packed with increasingly more hydrophobic chromatographic material are used in combination with mass spectrometry, is described. The ultimate aim was to gain increased sequence coverage from peptide mixtures derived from gel-separated proteins, in order to locate modified peptides. Graphite powder is described as an alternative to traditional

  10. Application of wall-stabilized plasma arc for the spectrometric determination of impurity elements in uranium yellow cake

    International Nuclear Information System (INIS)

    The application of a seeded wall-stabilized argon plasma arc as an excitation source for the emission spectrometric determination of some impurity elements in a sample of uranium yellow cake has been investigated. The sample was dissolved in nitric acid. Uranium was extracted from the sample solution using tributyl phosphate (TBP), and the aqueous solution was injected into the arc. The elements determined were Al, Ca, Fe, Mg, Mn, Mo, Sr and Zr. Limits of detection and precision of the technique are presented. The study of the influence of residual uranium in the nebulized solution on the intensity of spectral lines revealed that uranium concentrations up to 100 μg mL-1 have no significant interfering effect

  11. Desorption Electrospray Ionization (DESI) Mass Spectrometric Imaging of the Distribution of Rohitukine in the Seedling of Dysoxylum binectariferum Hook. F.

    Science.gov (United States)

    Mohana Kumara, Patel; Srimany, Amitava; Arunan, Suganya; Ravikanth, Gudasalamani; Uma Shaanker, Ramanan; Pradeep, Thalappil

    2016-01-01

    Ambient ionization mass spectrometric imaging of all parts of the seedling of Dysoxylum binectariferum Hook. f (Meliaceae) was performed to reconstruct the molecular distribution of rohitukine (Rh) and related compounds. The species accumulates Rh, a prominent chromone alkaloid, in its seeds, fruits, and stem bark. Rh possesses anti-inflammatory, anti-cancer, and immuno-modulatory properties. Desorption electrospray ionization mass spectrometry imaging (DESI MSI) and electrospray ionization (ESI) tandem mass spectrometry (MS/MS) analysis detected Rh as well as its glycosylated, acetylated, oxidized, and methoxylated analogues. Rh was predominantly distributed in the main roots, collar region of the stem, and young leaves. In the stem and roots, Rh was primarily restricted to the cortex region. The identities of the metabolites were assigned based on both the fragmentation patterns and exact mass analyses. We discuss these results, with specific reference to the possible pathways of Rh biosynthesis and translocation during seedling development in D. binectariferum. PMID:27362422

  12. Desorption Electrospray Ionization (DESI Mass Spectrometric Imaging of the Distribution of Rohitukine in the Seedling of Dysoxylum binectariferum Hook. F.

    Directory of Open Access Journals (Sweden)

    Patel Mohana Kumara

    Full Text Available Ambient ionization mass spectrometric imaging of all parts of the seedling of Dysoxylum binectariferum Hook. f (Meliaceae was performed to reconstruct the molecular distribution of rohitukine (Rh and related compounds. The species accumulates Rh, a prominent chromone alkaloid, in its seeds, fruits, and stem bark. Rh possesses anti-inflammatory, anti-cancer, and immuno-modulatory properties. Desorption electrospray ionization mass spectrometry imaging (DESI MSI and electrospray ionization (ESI tandem mass spectrometry (MS/MS analysis detected Rh as well as its glycosylated, acetylated, oxidized, and methoxylated analogues. Rh was predominantly distributed in the main roots, collar region of the stem, and young leaves. In the stem and roots, Rh was primarily restricted to the cortex region. The identities of the metabolites were assigned based on both the fragmentation patterns and exact mass analyses. We discuss these results, with specific reference to the possible pathways of Rh biosynthesis and translocation during seedling development in D. binectariferum.

  13. XMM-Newton and UV Detection of OVIII and Broad HI absorption towards PKS 0558-504: a possible WHIM filament

    CERN Document Server

    Nicastro, F; Fields, D; Conciatore, M L; Zappacosta, L; Elvis, M; Mathur, S; Papadakis, I

    2009-01-01

    We present the first likely X-ray detection associated with Broad HI Ly$\\beta$ (BLB) and Ly$\\alpha$ (BLA) absorbers, consistent with being a WHIM filament. The absorber lies along the line of sight to the nearby ($z=0.1372$) Seyfert 1 galaxy PKS 0558-504. The X-ray absorber is marginally detected in two independent XMM-Newton spectra of PKS 0558-504, with a combined single line statistical significance of 2.8$\\sigma$ (2.7$\\sigma$ and 1.2$\\sigma$ in the two spectra, respectively). When fitted with our self-consistent hybrid-photoionization WHIM models, the combined XMM-{\\em Newton} spectrum is consistent with the presence of an OVIII K$\\alpha$ absorber at $z=(0.117 \\pm 0.001)$, with log$T=6.56_{-0.17}^{+0.19}$ K, and logN$_H=(21.5 \\pm 0.3) (Z/Z_{0.01\\odot})^{-1}$ cm$^{-2}$. The lack of detection of associated OVI in the archival FUSE spectrum of PKS 0558-504, allows us to infer a tighter lower limit on the temperature, of log$T>6.52$ K (at 1$\\sigma$). The statistical sigificance of this single X-ray detection ...

  14. Real-time bilinear rotation decoupling in absorptive mode J-spectroscopy: Detecting low-intensity metabolite peak close to high-intensity metabolite peak with convenience.

    Science.gov (United States)

    Verma, Ajay; Baishya, Bikash

    2016-05-01

    "Pure shift" NMR spectra display singlet peak per chemical site. Thus, high resolution is offered at the cost of valuable J-coupling information. In the present work, real-time BIRD (BIlinear Rotation Decoupling) is applied to the absorptive-mode 2D J-spectroscopy to provide pure shift spectrum in the direct dimension and J-coupling information in the indirect dimension. Quite often in metabolomics, proton NMR spectra from complex bio-fluids display tremendous signal overlap. Although conventional J-spectroscopy in principle overcomes this problem by separating the multiplet information from chemical shift information, however, only magnitude mode of the experiment is practical, sacrificing much of the potential high resolution that could be achieved. Few J-spectroscopy methods have been reported so far that produce high-resolution pure shift spectrum along with J-coupling information for crowded spectral regions. In the present work, high-quality J-resolved spectrum from important metabolomic mixture such as tissue extract from rat cortex is demonstrated. Many low-intensity metabolite peaks which are obscured by the broad dispersive tails from high-intensity metabolite peaks in regular magnitude mode J-spectrum can be clearly identified in real-time BIRD J-resolved spectrum. The general practice of removing such spectral overlap is tedious and time-consuming as it involves repeated sample preparation to change the pH of the tissue extract sample and subsequent spectra recording.

  15. Ground-based demonstration of a CO2 remote sensor using a 1.57μm differential laser absorption spectrometer with direct detection

    Science.gov (United States)

    Sakaizawa, Daisuke; Kawakami, Shuji; Nakajima, Masakatsu; Sawa, Yosuke; Matsueda, Hidekazu

    2010-10-01

    A 1.57-μm laser remote sensor using differential absorption spectrometry is being developed as a candidate for the next space-based mission to observe atmospheric CO2 and/or other trace gases. The performance of the newly-developed active remote sensor has been evaluated for horizontal measurements and initial vertical measurements have been demonstrated. This study shows the results of in-house and field measurements to evaluate column-averaged CO2 mixing ratios. The in-house measurements demonstrated the instrumental response showing agreement within a correlation coefficient of 0.998 for a known CO2 density. Field measurements to evaluate horizontal and vertical column-averaged CO2 mixing ratio were made with a measured precision of 0.49% and 1.7%, respectively. The horizontal integration range was 2.1 km and the vertical range extended from the surface up to the cloud base at ~3 km with corresponding accumulation time of 25 min. Complementary measurements with a multi-positioned in-situ sensor along the observation path demonstrated that the mean horizontal column-averaged CO2 density agreed within the difference of 2.8 ppm of the atmospheric CO2 density.

  16. Real-time bilinear rotation decoupling in absorptive mode J-spectroscopy: Detecting low-intensity metabolite peak close to high-intensity metabolite peak with convenience

    Science.gov (United States)

    Verma, Ajay; Baishya, Bikash

    2016-05-01

    "Pure shift" NMR spectra display singlet peak per chemical site. Thus, high resolution is offered at the cost of valuable J-coupling information. In the present work, real-time BIRD (BIlinear Rotation Decoupling) is applied to the absorptive-mode 2D J-spectroscopy to provide pure shift spectrum in the direct dimension and J-coupling information in the indirect dimension. Quite often in metabolomics, proton NMR spectra from complex bio-fluids display tremendous signal overlap. Although conventional J-spectroscopy in principle overcomes this problem by separating the multiplet information from chemical shift information, however, only magnitude mode of the experiment is practical, sacrificing much of the potential high resolution that could be achieved. Few J-spectroscopy methods have been reported so far that produce high-resolution pure shift spectrum along with J-coupling information for crowded spectral regions. In the present work, high-quality J-resolved spectrum from important metabolomic mixture such as tissue extract from rat cortex is demonstrated. Many low-intensity metabolite peaks which are obscured by the broad dispersive tails from high-intensity metabolite peaks in regular magnitude mode J-spectrum can be clearly identified in real-time BIRD J-resolved spectrum. The general practice of removing such spectral overlap is tedious and time-consuming as it involves repeated sample preparation to change the pH of the tissue extract sample and subsequent spectra recording.

  17. Comparison of pigment content of paint samples using spectrometric methods

    Science.gov (United States)

    Trzcińska, Beata; Kowalski, Rafał; Zięba-Palus, Janina

    2014-09-01

    The aim of the paper was to evaluate the influence of pigment concentration and its distribution in polymer binder on the possibility of colour identification and paint sample comparison. Two sets of paint samples: one containing red and another one green pigment were prepared. Each set consisted of 13 samples differing gradually in the concentration of pigment. To obtain the sets of various colour shades white paint was mixed with the appropriate pigment in the form of a concentrated suspension. After solvents evaporation the samples were examined using spectrometric methods. The resin and main filler were identified by IR method. Colour and white pigments were identified on the base of Raman spectra. Colour of samples were compared based on Vis spectrometry according to colour theory. It was found that samples are homogenous (parameter measuring colour similarity ΔE < 3). The values of ΔE between the neighbouring samples in the set revealed decreasing linear function and between the first and following one - a logarithmic function.

  18. Spectrometric measurements of radioisotope activity in the thyroid

    Science.gov (United States)

    Osko, Jakub; Golnik, Natalia

    2008-01-01

    The results of measurements of iodine 131I and technetium 99mTc uptake in human thyroid, performed with scintillation or semiconductor detectors can exhibit a considerable uncertainty due to the differences in the thyroid position in the patient's neck. Basic physical laws of radiation attenuation and scattering show that the final shape of the registered spectrum should depends on the thyroid position in the neck and on the thickness of the tissue between the thyroid and the detector. The use of the spectrometric measuring method is proposed in this work for determination of the iodine gathering effective depth. The performed studies showed that the measurements results can be used for improving the accuracy of the iodine 131I activity in thyroid measurements and for selection of the group of patients for whom the anatomical position of the thyroid or the spatial distribution of the iodine gathering is much different than the standard one, assumed during the calibration of the counters. The results of the measurements were in agreement with Monte-Carlo calculations of the detector response. The method was used in routine monitoring of occupationally exposed persons, using the thyroid counter. A group of six persons with measurable internal contamination was selected and the measurements were performed on consecutive days, so the results could be registered at decreasing iodine activities in the thyroid. Larger series of measurements were performed at Brodno Regional Hospital in Warsaw, for a group of 95 patients after diagnostic administration of iodine 131I.

  19. Mass spectrometric study of the amipurimycin hexopyranosidic sugar moiety

    Science.gov (United States)

    Almoster Ferreira, M. A.; Borges, C.; Oliveira, M. C.; Pocsfalvi, G.; Rauter, A. P.; Fernandes, A. C.

    1997-11-01

    Amipurimycin is a natural nucleoside that displays a remarkable activity in vitro and in vivo against Pyricularia oryzae, which is responsible for the rice blast disease. Six important precursors for the synthesis of the Amipurimycin sugar moiety were prepared. In order to obtain structural information a mass spectrometric study of these compounds was performed using liquid secondary ion mass spectrometry (LSIMS) with high-energy collision-induced dissociation (CID) experiments on a four-sector instrument. Elimination of methanol is the preferential fragmentation path for five of the six protonated molecules, indicating that protonation plays an important role in the process, whilst for the other protonated molecule loss of water is the main fragmentation. Examination of the [M + Li]+ precursor ion spectra shows that loss of methanol does not occur in three of them, but in the other three gives rise to fairly abundant ions, indicating that in this case methanol elimination implies intramolecular hydrogen transfer, the resulting ion having a very stable structure.

  20. Surface acoustic wave nebulization facilitating lipid mass spectrometric analysis.

    Science.gov (United States)

    Yoon, Sung Hwan; Huang, Yue; Edgar, J Scott; Ting, Ying S; Heron, Scott R; Kao, Yuchieh; Li, Yanyan; Masselon, Christophe D; Ernst, Robert K; Goodlett, David R

    2012-08-01

    Surface acoustic wave nebulization (SAWN) is a novel method to transfer nonvolatile analytes directly from the aqueous phase to the gas phase for mass spectrometric analysis. The lower ion energetics of SAWN and its planar nature make it appealing for analytically challenging lipid samples. This challenge is a result of their amphipathic nature, labile nature, and tendency to form aggregates, which readily precipitate clogging capillaries used for electrospray ionization (ESI). Here, we report the use of SAWN to characterize the complex glycolipid, lipid A, which serves as the membrane anchor component of lipopolysaccharide (LPS) and has a pronounced tendency to clog nano-ESI capillaries. We also show that unlike ESI SAWN is capable of ionizing labile phospholipids without fragmentation. Lastly, we compare the ease of use of SAWN to the more conventional infusion-based ESI methods and demonstrate the ability to generate higher order tandem mass spectral data of lipid A for automated structure assignment using our previously reported hierarchical tandem mass spectrometry (HiTMS) algorithm. The ease of generating SAWN-MS(n) data combined with HiTMS interpretation offers the potential for high throughput lipid A structure analysis. PMID:22742654

  1. Functional proteomics with new mass spectrometric and bioinformatics tools

    International Nuclear Information System (INIS)

    A comprehensive range of mass spectrometric tools is required to investigate todays life science applications and a strong focus is on addressing the needs of functional proteomics. Application examples are given showing the streamlined process of protein identification from low femtomole amounts of digests. Sample preparation is achieved with a convertible robot for automated 2D gel picking, and MALDI target dispensing. MALDI-TOF or ESI-MS subsequent to enzymatic digestion. A choice of mass spectrometers including Q-q-TOF with multipass capability, MALDI-MS/MS with unsegmented PSD, Ion Trap and FT-MS are discussed for their respective strengths and applications. Bioinformatics software that allows both database work and novel peptide mass spectra interpretation is reviewed. The automated database searching uses either entire digest LC-MSn ESI Ion Trap data or MALDI MS and MS/MS spectra. It is shown how post translational modifications are interactively uncovered and de-novo sequencing of peptides is facilitated

  2. Multisphere neutron spectrometric system with thermoluminescence dosemeters: sensitive improvement.

    Science.gov (United States)

    Gregori, B; Papadópulos, S; Cruzate, J; Kunst, J J

    2002-01-01

    In this work, a neutron spectrometric system based on a set of moderating spheres with thermoluminescence detectors (TLD) is presented. The system at the Nuclear Regulatory Authority (ARN) Dosimetry Laboratory consists of 12 solid spheres made of high-density polyethylene (p = 0.95 g x cm(-3)), with diameters ranging from 2" to 12" and TLD sensitive to thermal and gamma radiation, namely TLD-600 and TLD-700, located at the centre of the spheres. The neutron response matrix for this Bonner Sphere Spectrometer (BSS) was calculated using the MCNP-IVB code and the library ENDF/B-VI in the energy range between thermal neutrons and 100 MeV. The neutron spectrum was obtained using the LOUH182 unfolding code. The improvement in sensitivity of the system is based on the election of a different heating cycle of the TLD that allows an increase in sensitivity by a factor of 2.6 compared with the standard laboratory treatment. The system response for the calibration with an Am-Be source is presented.

  3. A microchip electrophoresis-mass spectrometric platform with double cell lysis nano-electrodes for automated single cell analysis.

    Science.gov (United States)

    Li, Xiangtang; Zhao, Shulin; Hu, Hankun; Liu, Yi-Ming

    2016-06-17

    Capillary electrophoresis-based single cell analysis has become an essential approach in researches at the cellular level. However, automation of single cell analysis has been a challenge due to the difficulty to control the number of cells injected and the irreproducibility associated with cell aggregation. Herein we report the development of a new microfluidic platform deploying the double nano-electrode cell lysis technique for automated analysis of single cells with mass spectrometric detection. The proposed microfluidic chip features integration of a cell-sized high voltage zone for quick single cell lysis, a microfluidic channel for electrophoretic separation, and a nanoelectrospray emitter for ionization in MS detection. Built upon this platform, a microchip electrophoresis-mass spectrometric method (MCE-MS) has been developed for automated single cell analysis. In the method, cell introduction, cell lysis, and MCE-MS separation are computer controlled and integrated as a cycle into consecutive assays. Analysis of large numbers of individual PC-12 neuronal cells (both intact and exposed to 25mM KCl) was carried out to determine intracellular levels of dopamine (DA) and glutamic acid (Glu). It was found that DA content in PC-12 cells was higher than Glu content, and both varied from cell to cell. The ratio of intracellular DA to Glu was 4.20±0.8 (n=150). Interestingly, the ratio drastically decreased to 0.38±0.20 (n=150) after the cells are exposed to 25mM KCl for 8min, suggesting the cells released DA promptly and heavily while they released Glu at a much slower pace in response to KCl-induced depolarization. These results indicate that the proposed MCE-MS analytical platform may have a great potential in researches at the cellular level. PMID:27207575

  4. Determination of ultra trace amounts of bismuth in biological and water samples by electrothermal atomic absorption spectrometry (ET-AAS) after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Shemirani, Farzaneh; Baghdadi, Majid; Ramezani, Majid; Jamali, Mohammad Reza

    2005-04-04

    A new approach for a cloud point extraction electrothermal atomic absorption spectrometric method was used for determining bismuth. The aqueous analyte was acidified with sulfuric acid (pH 3.0-3.5). Triton X-114 was added as a surfactant and dithizone was used as a complexing agent. After phase separation at 50 deg. C based on the cloud point separation of the mixture, the surfactant-rich phase was diluted using tetrahydrofuran (THF). Twenty microliters of the enriched solution and 10 {mu}l of 0.1% (w/v) Pd(NO{sub 3}){sub 2} as chemical modifier were dispersed into the graphite tube and the analyte determined by electrothermal atomic absorption spectrometry. After optimizing extraction conditions and instrumental parameters, a preconcentration factor of 196 was obtained for a sample of only 10 ml. The detection limit was 0.02 ng ml{sup -1} and the analytical curve was linear for the concentration range of 0.04-0.60 ng ml{sup -1}. Relative standard deviations were <5%. The method was successfully applied for the extraction and determination of bismuth in tap water and biological samples (urine and hair)

  5. Diffuse interstellar absorption bands

    Institute of Scientific and Technical Information of China (English)

    XIANG FuYuan; LIANG ShunLin; LI AiGen

    2009-01-01

    The diffuse interstellar bands (DIBs) are a large number of absorption bands that are superposed on the interstellar extinction curve and are of interstellar origin. Since the discovery of the first two DIBs in the 1920s, the exact nature of DIBs still remains unclear. This article reviews the history of the detec-tions of DIBs in the Milky Way and external galaxies, the major observational characteristics of DIBs, the correlations or anti-correlations among DIBs or between DIBs and other interstellar features (e.g. the prominent 2175 Angstrom extinction bump and the far-ultraviolet extinction rise), and the proposed candidate carriers. Whether they are also present in circumstellar environments is also discussed.

  6. Diffuse interstellar absorption bands

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    The diffuse interstellar bands(DIBs) are a large number of absorption bands that are superposed on the interstellar extinction curve and are of interstellar origin. Since the discovery of the first two DIBs in the 1920s,the exact nature of DIBs still remains unclear. This article reviews the history of the detections of DIBs in the Milky Way and external galaxies,the major observational characteristics of DIBs,the correlations or anti-correlations among DIBs or between DIBs and other interstellar features(e.g. the prominent 2175 Angstrom extinction bump and the far-ultraviolet extinction rise),and the proposed candidate carriers. Whether they are also present in circumstellar environments is also discussed.

  7. A cold metal poor cloud traced by a weak MgII absorption at z~0.45. First detection of SiI, CaI and FeI in a QSO absorber

    CERN Document Server

    D'Odorico, Valentina

    2007-01-01

    We present the observations of a weak MgII absorption system detected at z~0.452 in the UVES high resolution spectrum of the QSO HE0001-2340. The weakest of the two MgII components forming the system shows associated absorptions due to SiI, CaI and FeI observed for the first time in a QSO spectrum. We investigate the nature of this absorber by comparing its properties with those of different classes of absorbers (weak MgII, Damped Ly-alpha systems and local interstellar clouds) and reproducing its ionization conditions with photoionization models. The observed absorber belongs to the class of weak MgII systems on the basis of its equivalent width, however the relative strength of commonly observed transitions deviates significantly from those of the above mentioned absorbers. A rough estimate of the probability to cross such a system with a QSO line of sight is P~0.03. The presence of rare neutral transitions suggests that the cloud is shielded by a large amount of neutral Hydrogen. A detailed comparison of t...

  8. Characterization of used lubricating oil by spectrometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Andressa Moreira de, E-mail: andressa@ctaa.embrapa.br [Embrapa Agroindustria de Alimentos, Guaratiba, Rio de Janeiro, RJ (Brazil); Correa, Sergio Machado [Faculdade de Engenharia. Universidade do Estado do Rio de Janeiro (UERJ), Resende, RJ (Brazil); Silva, Glauco Correa da [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2011-07-01

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-Elmer{sup R} OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX Shimadzu{sup R} model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100{mu}A, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics

  9. Characterization of used lubricating oil by spectrometric techniques

    International Nuclear Information System (INIS)

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-ElmerR OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX ShimadzuR model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100μA, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics Using GC

  10. 2DB: a Proteomics database for storage, analysis, presentation, and retrieval of information from mass spectrometric experiments

    Directory of Open Access Journals (Sweden)

    Hippler Michael

    2008-07-01

    Full Text Available Abstract Background The amount of information stemming from proteomics experiments involving (multi dimensional separation techniques, mass spectrometric analysis, and computational analysis is ever-increasing. Data from such an experimental workflow needs to be captured, related and analyzed. Biological experiments within this scope produce heterogenic data ranging from pictures of one or two-dimensional protein maps and spectra recorded by tandem mass spectrometry to text-based identifications made by algorithms which analyze these spectra. Additionally, peptide and corresponding protein information needs to be displayed. Results In order to handle the large amount of data from computational processing of mass spectrometric experiments, automatic import scripts are available and the necessity for manual input to the database has been minimized. Information is in a generic format which abstracts from specific software tools typically used in such an experimental workflow. The software is therefore capable of storing and cross analysing results from many algorithms. A novel feature and a focus of this database is to facilitate protein identification by using peptides identified from mass spectrometry and link this information directly to respective protein maps. Additionally, our application employs spectral counting for quantitative presentation of the data. All information can be linked to hot spots on images to place the results into an experimental context. A summary of identified proteins, containing all relevant information per hot spot, is automatically generated, usually upon either a change in the underlying protein models or due to newly imported identifications. The supporting information for this report can be accessed in multiple ways using the user interface provided by the application. Conclusion We present a proteomics database which aims to greatly reduce evaluation time of results from mass spectrometric experiments and enhance

  11. Absorption of light dark matter in semiconductors

    OpenAIRE

    Hochberg, Yonit; Lin, Tongyan; Zurek, Kathryn M.

    2016-01-01

    Semiconductors are by now well-established targets for direct detection of MeV to GeV dark matter via scattering off electrons. We show that semiconductor targets can also detect significantly lighter dark matter via an absorption process. When the dark matter mass is above the band gap of the semiconductor (around an eV), absorption proceeds by excitation of an electron into the conduction band. Below the band gap, multi-phonon excitations enable absorption of dark matter in the 0.01 eV to e...

  12. QSO Absorption Lines from QSOs

    CERN Document Server

    Bowen, D V; Ménard, B; Chelouche, D; Inada, N; Oguri, M; Richards, G T; Strauss, M A; Vanden Berk, Daniel E; York, D G; Bowen, David V.; Hennawi, Joseph F.; Menard, Brice; Chelouche, Doron; Inada, Naohisa; Oguri, Masamune; Richards, Gordon T.; Strauss, Michael A.; Berk, Daniel E. Vanden; York, Donald G.

    2006-01-01

    We present the results of a search for metal absorption lines in the spectra of background QSOs whose sightlines pass close to foreground QSOs. We detect MgII(2796,2803) absorption in Sloan Digital Sky Survey (SDSS) spectra of four z>1.5 QSOs whose lines of sight pass within 26-98 kpc of lower redshift (z~0.5-1.5) QSOs. The 100% [4/4 pairs] detection of MgII in the background QSOs is clearly at odds with the incidence of associated (z_abs ~ z_em) systems -- absorbers which exist towards only a few percent of QSOs. Although the quality of our foreground QSO spectra is not as high as the SDSS data, absorption seen towards one of the background QSOs clearly does not show up at the same strength in the spectrum of the corresponding foreground QSO. This implies that the absorbing gas is distributed inhomogeneously around the QSO, presumably as a direct consequence of the anisotropic emission from the central AGN. We discuss possible origins for the MgII lines, including: absorption by gas from the foreground QSO h...

  13. 基于耦合技术的单色光谱吸收法检测甲烷气体浓度%Based on the Optical fiber coupling technology of spectral absorption method to detect methane gas concentration

    Institute of Scientific and Technical Information of China (English)

    姜建国; 刘盈萱; 王源

    2014-01-01

    In allusion to flammable and explosive safety problems of electronic testing equipment in methane gas concentration and adjustable laser expensive prices, put forward an application of coupling technique of mono-chromatic spectrum tests to detect methane gas concentration. The choice of monochromatic light source is given based on, designed a monochromatic spectrum absorption detection device based on optical fiber coupling technolo-gy. Application of Matlab is proposed for methane gas concentration and two sets of data output voltage linear fit-ting. Through the output voltage to predict methane gas concentration, and exam the error of the predicted values and the real value. The experimental results show that optical fiber coupling technology was applied to monochromatic spectrum absorption method to detect methane gas concentration can be without power in real-time detection of methane gas concentration, error less than 2%.%针对电子检测装置在甲烷气体浓度检测时存在易燃易爆等安全隐患,本文提出了一种基于光纤耦合技术的单色光谱吸收法检测甲烷气体浓度的方案。给出了单色光源的选择依据,设计了基于光纤耦合技术的单色光谱吸收法检测装置,提出了应用Matlab对甲烷气体浓度与输出电压两组数据进行线性拟合。通过输出电压预测出甲烷气体浓度,并检测了预测值与真实值的误差。实验结果表明,将光纤耦合技术应用于单色光谱吸收法检测甲烷气体浓度,可以在无电力介入的情况下对甲烷气体浓度进行实时检测,误差不超过2%。

  14. D-xylose absorption

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003606.htm D-xylose absorption To use the sharing features on this page, please enable JavaScript. D-xylose absorption is a laboratory test to determine ...

  15. Single hair cocaine consumption monitoring by mass spectrometric imaging.

    Science.gov (United States)

    Porta, Tiffany; Grivet, Chantal; Kraemer, Thomas; Varesio, Emmanuel; Hopfgartner, Gérard

    2011-06-01

    Matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI-MSI) was used to image the distribution of cocaine and its metabolites in intact single hair samples from chronic users down to a concentration of 5 ng/mg. Acquisitions were performed in rastering mode, at a speed of 1 mm/s and in the selected reaction monitoring (SRM) mode on a MALDI triple quadrupole linear ion trap fitted with a high repetition rate laser (1 kHz). Compared to traditional methods based on LC-MS/MS or GC-MS(/MS) which require to segment the hair to obtain spatial resolution, MALDI-MSI, with a straightforward sample preparation beforehand, allowed obtaining a spatial resolution of 1 mm and thus the chronological information about cocaine consumption contained in a single intact hair over several months could be monitored. The analysis time of an intact single hair sample of 6 cm is approximately of 6 min. Cocaine and its metabolites benzoylecgonine, ethylcocaine, and norcocaine were investigated in nine sets of hair samples for forensic purposes. The analyses were accomplished by spraying α-cyano-4-hydroxycinnamic acid (CHCA), 4-chloro-α-cyano-cinnamic acid (Cl-CCA), or (E)-2-cyano-3-(naphthalen-2-yl)acrylic acid (NpCCA) as MALDI matrices. We also propose a rapid strategy for sensitive confirmatory analyses with both MS/MS and MS(3) experiments performed directly on intact hair samples. Since only part of the hair strand is analyzed, additional analyses are possible at any time on the remaining hair from the strand. PMID:21510611

  16. Hydrogen--deuterium exchange in water vapor: the mass spectrometric sensitivities and the equilibrium constant

    Energy Technology Data Exchange (ETDEWEB)

    Pyper, J.W.; Dupzyk, R.J.; Friesen, R.D.; Bernasek, S.L.; May, C.A.; Echeverria, A.W.; Tolman, L.F.

    1976-04-21

    The equilibrium constant, K/sub HDO/, for the reaction H/sub 2/O + D/sub 2/O = 2HDO can be expressed as an intensity ratio, I, measured mass spectrometrically, times a sensitivity ratio, S, measured in mass spectrometric calibration experiments. The latter is difficult to measure and previously was assumed to be unity. The 2.4 percent discrepancy between K's from theoretical calculations and direct mass spectrometric measurements might be explained by another value of S. An indirect measurement of S using a pulsed-molecular beam quadrupole mass filter that has a unique three-chamber, three-leak gas inlet system is reported. The results show the sensitivities are probably equal and therefore S = 1. Systematic errors were found in the procedure, however, which precluded an unambiguous test of the theory.

  17. Modular mass spectrometric tool for analysis of composition and phosphorylation of protein complexes.

    Directory of Open Access Journals (Sweden)

    Justin D Blethrow

    Full Text Available The combination of high accuracy, sensitivity and speed of single and multiple-stage mass spectrometric analyses enables the collection of comprehensive sets of data containing detailed information about complex biological samples. To achieve these properties, we combined two high-performance matrix-assisted laser desorption ionization mass analyzers in one modular mass spectrometric tool, and applied this tool for dissecting the composition and post-translational modifications of protein complexes. As an example of this approach, we here present studies of the Saccharomyces cerevisiae anaphase-promoting complexes (APC and elucidation of phosphorylation sites on its components. In general, the modular concept we describe could be useful for assembling mass spectrometers operating with both matrix-assisted laser desorption ionization (MALDI and electrospray ionization (ESI ion sources into powerful mass spectrometric tools for the comprehensive analysis of complex biological samples.

  18. Calcium absorption and achlorhydria

    International Nuclear Information System (INIS)

    Defective absorption of calcium has been thought to exist in patients with achlorhydria. The author compared absorption of calcium in its carbonate form with that in a pH-adjusted citrate form in a group of 11 fasting patients with achlorhydria and in 9 fasting normal subjects. Fractional calcium absorption was measured by a modified double-isotope procedure with 0.25 g of calcium used as the carrier. Mean calcium absorption (+/- S.D.) in the patients with achlorhydria was 0.452 +/- 0.125 for citrate and 0.042 +/- 0.021 for carbonate (P less than 0.0001). Fractional calcium absorption in the normal subjects was 0.243 +/- 0.049 for citrate and 0.225 +/- 0.108 for carbonate (not significant). Absorption of calcium from carbonate in patients with achlorhydria was significantly lower than in the normal subjects and was lower than absorption from citrate in either group; absorption from citrate in those with achlorhydria was significantly higher than in the normal subjects, as well as higher than absorption from carbonate in either group. Administration of calcium carbonate as part of a normal breakfast resulted in completely normal absorption in the achlorhydric subjects. These results indicate that calcium absorption from carbonate is impaired in achlorhydria under fasting conditions. Since achlorhydria is common in older persons, calcium carbonate may not be the ideal dietary supplement

  19. Mass spectrometric analysis of electrophoretically separated allergens and proteases in grass pollen diffusates

    Directory of Open Access Journals (Sweden)

    Geczy Carolyn L

    2003-09-01

    Full Text Available Abstract Background Pollens are important triggers for allergic asthma and seasonal rhinitis, and proteases released by major allergenic pollens can injure airway epithelial cells in vitro. Disruption of mucosal epithelial integrity by proteases released by inhaled pollens could promote allergic sensitisation. Methods Pollen diffusates from Kentucky blue grass (Poa pratensis, rye grass (Lolium perenne and Bermuda grass (Cynodon dactylon were assessed for peptidase activity using a fluorogenic substrate, as well as by gelatin zymography. Following one- or two-dimensional gel electrophoresis, Coomassie-stained individual bands/spots were excised, subjected to tryptic digestion and analysed by mass spectrometry, either MALDI reflectron TOF or microcapillary liquid chromatography MS-MS. Database searches were used to identify allergens and other plant proteins in pollen diffusates. Results All pollen diffusates tested exhibited peptidase activity. Gelatin zymography revealed high Mr proteolytic activity at ~ 95,000 in all diffusates and additional proteolytic bands in rye and Bermuda grass diffusates, which appeared to be serine proteases on the basis of inhibition studies. A proteolytic band at Mr ~ 35,000 in Bermuda grass diffusate, which corresponded to an intense band detected by Western blotting using a monoclonal antibody to the timothy grass (Phleum pratense group 1 allergen Phl p 1, was identified by mass spectrometric analysis as the group 1 allergen Cyn d 1. Two-dimensional analysis similarly demonstrated proteolytic activity corresponding to protein spots identified as Cyn d 1. Conclusion One- and two-dimensional electrophoretic separation, combined with analysis by mass spectrometry, is useful for rapid determination of the identities of pollen proteins. A component of the proteolytic activity in Bermuda grass diffusate is likely to be related to the allergen Cyn d 1.

  20. Study on Experiment of Absorption Spectroscopy Detection of Pesticide Residues of Carbendazim in Orange Juice%橙汁中多菌灵农药残留吸收光谱特征研究

    Institute of Scientific and Technical Information of China (English)

    季仁东; 陈梦岚; 赵志敏; 朱星玥; 王乐新; 刘全金

    2014-01-01

    coefficient was 0 .996 ,and the recovery was :81% ~102% .According to the regression model ,we can ob-tain the amount of carbendazim pesticide residues in orange juice .It was verified that the method of using ultraviolet-visible ab-sorption spectra was feasible to detect the carbendazim residues in orange juice .The result proved that it is possible to detect pesticide residues of carbendazim in orange juice ,and it can meet the needs of rapid analysis .This study provides a new way for the detection of pesticide residues .

  1. Variability of calcium absorption

    International Nuclear Information System (INIS)

    Variability in calcium absorption was estimated in three groups of normal subjects in whom Ca absorption was measured by standard isotopic-tracer methods at interstudy intervals ranging from 1 to 4 mo. Fifty absorption tests were performed in 22 subjects. Each was done in the morning after an overnight fast with an identical standard breakfast containing a Ca load of approximately 250 mg. Individual fractional absorption values were normalized to permit pooling of the data. The coefficient of variation (CVs) for absorption for the three groups ranged from 10.57 to 12.79% with the size of the CV increasing with interstudy duration. One other published study presenting replicate absorption values was analyzed in a similar fashion and was found to have a CV of absorption of 9.78%. From these data we estimate that when the standard double-isotope method is used to measure Ca absorption there is approximately 10% variability around any given absorption value within an individual human subject and that roughly two-thirds of this represents real biological variability in absorption

  2. 微电纯化装置用于重组人促红细胞生成素的质谱分析前样品快速除盐%Rapid Desalting of Recombinant Human Erythropoietin Sample by Microelectro Purification Device for Mass Spectrometric Detection

    Institute of Scientific and Technical Information of China (English)

    庞楠楠; 周宇; 白玉; 廖杰; 刘虎威

    2011-01-01

    Microelectro purification device (MEPD) constructed by our laboratory could obtain online desalting of recombinant human erythropoietin (rhEPO) in 2 min with high efficiency. Electrospray mass spectrometry with positive ion mode was used for the detection. Compared with traditional methods, such as gradient elution by C18-reversed phase liquid chromatography (150 mm × 4. 6 mm,5 μm) as well as ultra-filtration, MEPD could further enhance the signal to noise ratio of rhEPO and the detection sensitivity. It could also shorten the analysis time dramatically. This simple and rapid method could be a promising pretreatment candidate for the rhEPO analysis of mass spectrometry.%利用实验室构建的微电纯化装置(Microelectro purification device,MEPD),采用电喷雾质谱正离子模式检测,在2min之内实现重组人促红细胞生成素(recombinant human erythropoietin,rhEPO)的在线脱盐,同时和传统的C18色谱柱(150 mm×4.6 mm,5 μm)梯度洗脱以及超滤管除盐结果进行比较.利用MEPD除盐后,rhEPO特征离子信噪比增加,检测灵敏度明显提高,操作时间大大缩短.本方法简单、快速,可作为质谱分析rhEPO样品的前处理方法.

  3. Absorption of light dark matter in semiconductors

    CERN Document Server

    Hochberg, Yonit; Zurek, Kathryn M

    2016-01-01

    Semiconductors are by now well-established targets for direct detection of MeV to GeV dark matter via scattering off electrons. We show that semiconductor targets can also detect significantly lighter dark matter via an absorption process. When the dark matter mass is above the band gap of the semiconductor (around an eV), absorption proceeds by excitation of an electron into the conduction band. Below the band gap, multi-phonon excitations enable absorption of dark matter in the 0.01 eV to eV mass range. Energetic dark matter particles emitted from the sun can also be probed for masses below an eV. We show that the reach for absorption of a relic kinetically mixed dark photon or pseudoscalar in semiconductors such as germanium or silicon can exceed current astrophysical and terrestrial constraints, with only a moderate exposure.

  4. Thermal ionization mass spectrometric study of U-Pu-O system

    International Nuclear Information System (INIS)

    First inference from a thermal ionization mass spectrometric study of samples corresponding to the ternary U-Pu-O system, especially if high surface ionization temperatures are employed, is likely to be at variance with that from equilibrium vaporization thermodynamic studies, that the atomic species U and Pu dominate the vapor phase

  5. Gas Chromatographic Mass Spectrometric Determination of Myo-inositol in Humans Utilizing a Deuterated Internal Standard

    DEFF Research Database (Denmark)

    Andersen, Jan Rud; Larsen, Elfinn; Harbo, Helge;

    1982-01-01

    , was added as internal standard to the samples at an early stage in the analytical procedure. After separation and derivatization to the hexa-acetate, the gas chromatographic mass spectrometric analysis was carried out. A 25 m fused silica capillary column coated with methyl silicone was used, and the ions...

  6. Electrothermal atomic absorption spectrometric determination of lithium, sodium, potassium and copper in uranium without preliminary chemical separation

    International Nuclear Information System (INIS)

    Graphite furnace atomization is used for the direct determination of Li (0.25-4 ppm), Na (8-70 ppm), K (20-300 ppm) and Cu (0.5-25 ppm) in uranium dissolved in nitric acid, with relative standard deviations of 4-9%. Only iron seriously depresses the signals from the alkali metals. (Auth.)

  7. Biosorption of platinum and palladium for their separation/preconcentration prior to graphite furnace atomic absorption spectrometric determination

    International Nuclear Information System (INIS)

    Inexpensive baker's yeast Saccharomyces cerevisiae and green algae Chlorella vulgaris, either free or immobilized on silica gel have been shown to selectively accumulate platinum and palladium from water samples in acidic medium (pH 1.6-1.8). Optimization of conditions of metals biosorption (sample pH, algae and yeast masses, adsorption time, temperature) was performed in batch mode. The procedure of matrix separation based on biosorption of platinum and palladium on algae C. vulgaris covalently immobilized on silica gel in flow mode was developed. The use of algae in flow procedure offers several advantages compared with its use in the batch mode. The procedure shows better reproducibility (-1 thiourea in 1 mol l-1 hydrochloric acid. The influence of thiourea on analytical signals of examined metals during GFAAS determination is discussed. The procedure has been applied for separation of noble metals from tap and waste water samples spiked with platinum and palladium

  8. Separation and preconcentration of ultratrace levels of cadmium(II) in a sequential injection (SI) system with a PTFE packed column as a mimic sequential injection lab-on-valve (SI-LOV) system with renewable column employing detection by electrothermal atomic absorption spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr;

    cadmium(II) by detection with electrothermal atomic absorption spectrometry (ETAAS). The non-charged complex formed between the analyste and the chelating reagent diethyldithiophosphate (DDPA) was selectively adsorbed on the surface of the PTFE beads and eluted by ethanol before being directed to the...

  9. Development of a miniature dielectric barrier discharge–optical emission spectrometric system for bromide and bromate screening in environmental water samples

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •Dielectric barrier discharge (DBD) is for the first time used as a radiation source for the excitation of bromine and its emission. •A DBD–optical emission spectrometric (OES) system was developed for the detection of bromide and bromate. •The DBD–OES system has been demonstrated by screening trace bromide and bromate in a series of environmental water samples. -- Abstract: Dielectric barrier discharge (DBD) at atmospheric pressure provides an efficient radiation source for the excitation of bromine and it is used for the first time for optical emission spectrometric (OES) detection of bromide and bromate. A portable DBD–OES system is developed for screening potential pollution from bromide and bromate in environmental waters. Bromide is on-line oxidized to bromine for in-situ generation of volatile bromine. Meanwhile, a helium stream carries bromine into the DBD micro-plasma for its excitation at a discharging voltage of 3.7 kV and optical emission spectrometric detection with a QE65000 charge-coupled device (CCD) spectrometer in the near-infrared spectral region. Similarly, the quantification of bromate is performed by its pre-reduction into bromide and then oxidized to bromine. The spectral characteristics and configuration of the DBD micro-plasma excitation source in addition to the oxidation vapor generation of bromine have been thoroughly investigated. With a sampling volume of 1 mL, a linear range of 0.05–10.0 mg L−1 is obtained with a detection limit of 0.014 mg L−1 by measuring the emission at 827 nm. A precision of 2.3% is achieved at 3 mg L−1 bromide. The system is validated by bromine detection in certified reference material of laver (GBW10023) at mg L−1 level, giving rise to satisfactory agreement. In addition, it is further demonstrated by screening trace bromide and bromate as well as spiking recoveries in a series of environmental water samples

  10. Absorption, luminescence, and scattering of single nano-objects

    NARCIS (Netherlands)

    Yorulmaz, Mustafa

    2013-01-01

    We study the technique of photothermal microscopy by which we can detect single nano-objects by their absorption at room temperature. We optimize the sensitivity of this technique and demonstrate the first optical detection of a single molecule by its absorption at room temperature. Moreover, we com

  11. Detection of the magnetic and electric transitions by electron paramagnetic resonance and low-field microwave absorption in the magnetoelectric Pb(Fe{sub 0.5}Ta{sub 0.5})O{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Alvarez, G., E-mail: memodin@yahoo.co [Departamento de Fisica, ESFM-IPN, U.P. Adolfo Lopez Mateos Edificio 9, Av. Instituto Politecnico Nacional S/N, San Pedro Zacatenco, Mexico DF 07738 (Mexico); Montiel, H. [Departamento de Tecnociencias, Centro de Ciencias Aplicadas y Desarrollo Tecnologico de la Universidad Nacional Autonoma de Mexico, Apartado Postal 70-360, Mexico DF 04510 (Mexico); Pena, J.A.; Castellanos, M.A. [Facultad de Quimica, Universidad Nacional Autonoma de Mexico, Cd. Universitaria, Mexico DF 04510 (Mexico); Zamorano, R. [Departamento de Fisica, ESFM-IPN, U.P. Adolfo Lopez Mateos Edificio 9, Av. Instituto Politecnico Nacional S/N, San Pedro Zacatenco, Mexico DF 07738 (Mexico)

    2010-10-22

    Graphical abstract: Display Omitted Research highlights: {yields} LFMA spectra showed straight lines with positive slope and non-hysteretic traces. {yields} The spectral changes for the plot of the slope vs. temperature give evidence of magnetic and electric orderings, with a very high detection sensibility. - Abstract: An electron paramagnetic resonance (EPR) study of Pb(Fe{sub 0.5}Ta{sub 0.5})O{sub 3} powder samples in perovskite-type structure at X-band (8.8-9.8 GHz), in the 120-300 K temperature range, is presented. For all the temperatures, the EPR spectra show a single broad line attributable to Fe{sup 3+} ions. The onset of the ferro-paraelectric and antiferro-paramagnetic transitions has been determined from the temperature dependence of parameters deduced from the EPR spectra: the peak-to-peak linewidth ({Delta}H{sub pp}), the resonance field (H{sub res}) and the integrated intensity (I{sub EPR}). Low-field microwave absorption (LFMA) is used to give further knowledge on this material; where this technique also gives evidence of the magnetic and electric orders.

  12. MASERATI: a new rocket-borne diode laser absorption spectrometer for in-situ measurement of trace gases in the middle and upper atmosphere; MASERATI: Ein neues raketengetragenes Diodenlaser-Absorptionsspektrometer zur in situ-Messung von Spurengasen in der mittleren und oberen Atmosphaere

    Energy Technology Data Exchange (ETDEWEB)

    Lucke, H. von

    1999-09-01

    MASERATI (middle atmosphere spectrometric experiment on Rockets for the analysis of trace gas influences) is the first rocket-borne tunable diode laser absorption spectrometer (TDLAS). It was developed to measure water vapor and carbon dioxide in the altitude range from 50 to 90 km and 120 km, respectively. Infrared absorption spectroscopy using two laser diodes is applied to measure both trace gases simultaneously. The laser beams are sent into an open multiple-pass absorption setup mounted on top of the sounding rocket. High sensitivity is achieved by means of frequency modulation and lock-in techniques. The results of several tests performed in the laboratory demonstrate that the instrument is capable of detecting relative absorbances down to 10{sup -4} - 10{sup -5} when integrating spectra for 1 s. Two almost identical MASERATI instruments have been built and launched on sounding rockets from the Andoeya rocket range (69 N, 16 E) in northern Norway during winter 1997/98. The results of these flights demonstrate that MASERATI is a new suitable tool for in situ studies of the mesosphere and lower thermosphere. (orig.)

  13. Mass spectrometric analysis of the marine lipophilic biotoxins pectenotoxin-2 and okadaic acid by four different types of mass spectrometers.

    Science.gov (United States)

    Gerssen, Arjen; Mulder, Patrick; van Rhijn, Hans; de Boer, Jacob

    2008-08-01

    The performances of four different mass spectrometers [triple-quadrupole (TQ), time-of-flight (ToF), quadrupole ToF (Q-ToF) and ion trap (IT)] for the detection of the marine lipophilic toxins pectenotoxin-2 (PTX2) and okadaic acid (OA) were investigated. The spectral data obtained with the different mass spectrometric analyzers were used to propose fragmentation schemes for PTX2 in the positive electrospray mode and for OA in the negative electrospray mode. TQ data were used to obtain product ions, while ToF and Q-ToF-MS produced accurate mass data of the precursor ion and product ions, respectively. IT data provided a better understanding of the fragmentation pathways using MS(n) experiments. With respect to analytical performance, all four mass analyzers showed a good linearity (R(2) > 0.97) and repeatability (CV < 20%). Detection limits (LoDs) (S/N = 3) were the lowest on triple-quad MS: 12.2 and 2.9 pg on-column for PTX2 and OA, respectively.

  14. Nutrition and magnesium absorption.

    NARCIS (Netherlands)

    Brink, E.J.

    1992-01-01

    The influence of various nutrients present in dairy products and soybean-based products on absorption of magnesium has been investigated. The studies demonstrate that soybean protein versus casein lowers apparent magnesium absorption in rats through its phytate component. However, true magnesium abs

  15. Application of mass spectrometric techniques for the trace analysis of short-lived iodine-containing volatiles emitted by seaweed.

    Science.gov (United States)

    Kundel, Michael; Thorenz, Ute R; Petersen, Jan H; Huang, Ru-Jin; Bings, Nicolas H; Hoffmann, Thorsten

    2012-04-01

    Knowledge of the composition and emission rates of iodine-containing volatiles from major widespread seaweed species is important for modeling the impact of halogens on gas-phase atmospheric chemistry, new particle formation, and climate. In this work, we present the application of mass spectrometric techniques for the quantification of short-lived iodine-containing volatiles emitted by eight different seaweeds from the intertidal zone of Helgoland, Germany. A previously developed online time-of-flight aerosol mass spectrometric method was used to determine I(2) emission rates and investigate temporally resolved emission profiles. Simultaneously, iodocarbons were preconcentrated on solid adsorbent tubes and quantified offline using thermodesorption-gas chromatography-mass spectrometry. The total iodine content of the seaweeds was determined using microwave-assisted tetramethylammonium hydroxide extraction followed by inductively coupled-plasma mass spectrometry analysis. The highest total iodine content was found in the Laminariales, followed by the brown algae Ascophyllum nodosum, Fucus vesiculosus, Fucus serratus, and both red algae Chondrus crispus and Delesseria sanguinea. Laminariales were found to be the strongest I(2) emitters. Time series of the iodine release of Laminaria digitata and Laminaria hyperborea showed a strong initial I(2) emission when first exposed to air followed by an exponential decline of the release rate. For both species, I(2) emission bursts were observed. For Laminaria saccharina und F. serratus, a more continuous I(2) release profile was detected, however, F. serratus released much less I(2). A. nodosum and F. vesiculosus showed a completely different emission behavior. The I(2) emission rates of these species were slowly increasing with time during the first 1 to 2 h until a more or less stable I(2) emission rate was reached. The lowest I(2) emission rates were detected for the red algae C. crispus and D. sanguinea. Total iodocarbon

  16. Arsenic and antimony determination in refined and unrefined table salts by means of hydride generation atomic absorption spectrometry--comparison of sample decomposition and determination methods

    OpenAIRE

    AKSUNER, Nur; TİRTOM, Vedia Nüket; HENDEN, Emür

    2011-01-01

    An evaluation was made of different digestion methods for the determination of arsenic and antimony in table salt samples prior to hydride generation atomic absorption spectrometric analysis. Microwave acid digestion, classical wet digestion, dry ashing, and fusion were applied to the decomposition of salt samples and optimum conditions were investigated. Samples were decomposed by changing heating time, digestion techniques, and the amount and composition of acid, and then the concen...

  17. The accuracy of X-ray fluorescence spectrometric determination of Rb and Sr contents in rock sample

    International Nuclear Information System (INIS)

    It is shown that application of the Compton scattering method in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide element contents at an accuracy level +- 1 %

  18. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal to determine compliance with specifications.

  19. Flow injection determination of copper in mussels by flame atomic absorption spectrometry after on-line continuous ultrasound-assisted extraction

    Science.gov (United States)

    Moreno-Cid, A.; Yebra, M. C.

    2002-05-01

    Copper was extracted on-line from solid mussel samples by a simple and rapid continuous ultrasound-assisted extraction system (CUES). The CUES is connected to a flow injection manifold, which permits the on-line flame atomic absorption spectrometric determination of copper. The manifold is simple and the copper signal was obtained for a volume of 250 μl of acid leachate injected into an ultrapure water carrier stream. An experimental design was used for the optimization of the continuous leaching procedure. Compared to off-line ultrasonic-assisted extraction methods, sonication time is reduced by factors of 6-12, the leaching takes place at room temperature (20 °C), and the analysis time is reduced because centrifugation was not necessary to separate the liquid phase. The method allowed a total sampling frequency of 11 samples h -1, with a relative standard deviation for the complete procedure of 2.7% (for a sample containing 2.0 μg g -1 copper (wet mass, n=11). The limit of detection was 0.06 μg g -1 (wet mass) for 30 mg of sample. The analytical procedure was verified for a reference standard material (TORT-1). The analytical procedure was applied to mussel samples from Galicia (Spain).

  20. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry in water samples

    Directory of Open Access Journals (Sweden)

    Arpa Şahin Ç.

    2013-04-01

    Full Text Available A simple, rapid and inexpensive solidified floating organic drop microextraction (SFODME and flow injection flame atomic absorption spectrometric determination (FI-FAAS method for copper was developed. 3-amino-7-dimethylamino-2-methylphenazine (Neutral red, NR was used as the complexing agent. Several factors affecting the microextraction efficiency, such as, pH, NR and sodium dodecylbenzenesulfonate (SDBS concentration, extraction time, stirring rate, and temperature were investigated and optimized. Under optimized experimental conditions an enrichment factor of 541 was obtained for 100 mL of sample solution. The calibration graph was linear in the range of 0.5 – 20.0 ng mL–1 and the limit of detection (3s was 0.18 ng mL–1, the limit of quantification (10s was 0.58 ng mL–1. The relative standard deviation (RSD for 10 replicate measurements of 10 ng mL–1 copper was 2.7%. The developed method was successfully applied to the extraction and determination of copper in different certified reference materials (Estuarine water, Slew 3 and fortified water, TM 23.2 and real water samples and satisfactory results were obtained.

  1. Coprecipitation of trace elements with Ni2+/2-Nitroso-1-naphthol-4-sulfonic acid and their determination by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ni2+/2-Nitroso-1-naphthol-4-sulfonic acid precipitate was used for the coprecipitation of Co, Pb, Cu, Fe and Zn prior to their flame atomic absorption spectrometric (FAAS) determinations in environmental samples. The precipitate could be easily dissolved with concentrated nitric acid. The recovery values for analyte ions were higher than 95%. The parameters including pH, sample volume, centrifuge time, amounts of nickel and matrix effects were optimized for the quantitative recoveries of the analytes. The relative standard deviations of cobalt, lead, copper, iron and zinc were found 4.5, 5.7, 3.8, 6.1 and 7.5%, respectively. The limit of detection was calculated as 1.05, 2.67, 1.30, 1.38, and 0.50 μg L-1 for cobalt, lead, copper, iron and zinc. The validation of the procedure was checked by the analysis of IAEA 336 lichen and SLRS 4 Riverine water standard reference materials were analyzed with satisfactory results. The presented coprecipitation procedure was successfully applied to some environmental samples for determination of analyte ions.

  2. Antimony in drinking water, red blood cells, and serum: development of analytical methodology using transversely heated graphite furnace atomization-atomic absorption spectrometry.

    Science.gov (United States)

    Subramanian, K S; Poon, R; Chu, I; Connor, J W

    1997-05-01

    An atomic absorption spectrometric (AAS) method has been developed for determining microg/L levels of Sb in samples of water and blood. The AAS method is based on the concept of stabilized temperature platform furnace atomization (STPF) realized through the use of a transversely heated graphite atomizer (THGA) furnace, longitudinal Zeeman-effect background correction, and matrix modification with palladium nitrate-magnesium nitrate-nitric acid. The method of standard additions is not mandatory. The detection limit (3 standard deviations of the blank) is 2.6 microg Sb/L for the water, red blood cells (RBCs), and serum samples. Data are presented on the degree of accuracy and precision. The THGA-AAS method is simple, fast, and contamination-free because the entire operation from sampling to AAS measurement is carried out in the same tube. The method has been applied to the determination of Sb in some leachate tap water samples derived from a static copper plumbing system containing Sn/Sb solders, and in small samples (0.5 ml) of RBCs and serum derived from rats given Sb-supplemented drinking water. PMID:9175512

  3. Determination of trace elements in dolomite and gypsum by atomic absorption spectrometry: overcoming the matrix interference by flotation separation

    Science.gov (United States)

    Stafilov, Trajče; Zendelovska, Dragica; Pavlovska, Gorica; Čundeva, Katarina

    2002-05-01

    The interferences of Ca and Mg as matrix elements in dolomite and gypsum on Ag, Cd, Cr, Mn, Tl and Zn absorbances during their electrothermal atomic absorption spectrometric (ETAAS) determination are investigated. The results reveal that Ca and Mg do not interfere on Zn and Mn, tend to decrease absorbances of Ag, Cd and Cr, while Tl suffers the most significant influence. A flotation separation method is proposed to eliminate matrix interferences. Hydrated iron(III) oxide, Fe 2O 3· xH 2O, and iron(III) hexamethylenedithiocarbamate, Fe(HMDTC) 3, are applied as flotation collectors. The influence of hydrophobic dithiocarbamate anion, HMDTC, on flotation recoveries of each analyte is studied. The most suitable concentrations of dolomite and gypsum solutions for flotation are determined. To avoid flotation suppression due to the reaction of Ca 2+ and Mg 2+ with surfactant ions, a fit foaming agent was selected. The elements present in dolomite and gypsum as traces have been analyzed by ETAAS. Their ETAAS limits of detection following flotation are found to be 0.021 μg·g -1 for Ag, 0.019 μg·g -1 for Cd, 0.014 μg·g -1 for Cr and 0.11 μg·g -1 for Tl. The determination of Mn and Zn can be performed by flame AAS (FAAS). The limit of detection for Mn is 1.5 μg·g -1, while for Zn 0.8 μg·g -1.

  4. Molecular absorption in transition region spectral lines

    CERN Document Server

    Schmit, Donald; Ayres, Thomas; Peter, Hardi; Curdt, Werner; Jaeggli, Sarah

    2014-01-01

    Aims: We present observations from the Interface Region Imaging Spectrograph (IRIS) of absorption features from a multitude of cool atomic and molecular lines within the profiles of Si IV transition region lines. Many of these spectral lines have not previously been detected in solar spectra. Methods: We examined spectra taken from deep exposures of plage on 12 October 2013. We observed unique absorption spectra over a magnetic element which is bright in transition region line emission and the ultraviolet continuum. We compared the absorption spectra with emission spectra that is likely related to fluorescence. Results: The absorption features require a population of sub-5000 K plasma to exist above the transition region. This peculiar stratification is an extreme deviation from the canonical structure of the chromosphere-corona boundary . The cool material is not associated with a filament or discernible coronal rain. This suggests that molecules may form in the upper solar atmosphere on small spatial scales...

  5. 'Age' determination of irradiated materials utilizing inductively coupled plasma mass spectrometric (ICP-MS) detection

    International Nuclear Information System (INIS)

    A gas pressurized extraction chromatography (GPEC) system has been developed to perform elemental separations on radioactive samples to determine total and isotopic compositions of Cs and Ba from an irradiated salt sample, fuel sample and two sealed radiation sources. The GPEC system employs compressed nitrogen to move liquid through the system, compared to gravity or pumped liquids that are typically used for separations. A commercially available Sr-ResinTM was used to perform the separation for the above mentioned analytes. A 1% acetic acid solution was determined to be the best extractant for Ba. A flow rate of 0.1 mL/min was determined to be optimal for the separation of Ba. Complete recovery of the Cs and Ba was achieved, within the systematic uncertainties of the experiments. (author)

  6. Pressurised Fluid Extraction of Bioactive Species in Tree Barks : Analysis using Hyphenated Electrochemical Mass Spectrometric Detection

    OpenAIRE

    Co, Michelle

    2010-01-01

    Analytical chemistry has developed throughout time to meet current needs. At present, the interest in biorefinery is growing, due to environmental awareness and the depletion of fossil resources. Biomass from agricultural and forestry industries has proven to be excellent raw material for different processes. Biorefinering valuable species such as bioactive species from biomass, without compromising the primary process of the biomass is highly desirable. Pressurised fluid extraction (PFE) usi...

  7. Photochemical vapor generation of lead for inductively coupled plasma mass spectrometric detection

    Science.gov (United States)

    Duan, Hualing; Zhang, Ningning; Gong, Zhenbin; Li, Weifeng; Hang, Wei

    2016-06-01

    Photochemical vapor generation (PCVG) of lead was successfully achieved with a simplified and convenient system, in which only low molecular weight organic acid and a high-efficiency photochemical reactor were needed. The reactor was used to generate lead volatile species when a solution of lead containing a small amount of low molecular weight organic acid was pumped through. Several factors, including the concentration of acetic acid, the concentration of hydrochloride acid, and the irradiation time of UV light were optimized. Under the optimal conditions, including the addition of 0.90% (v/v) acetic acid and 0.03% (v/v) hydrochloride acid, and irradiation time of 28 s, intense and repeatable signal of lead volatile species was successfully obtained and identified with inductively coupled plasma mass spectrometry (ICPMS). In addition, the effects from inorganic anions and transition metal ions, including Cl-, NO3-, SO42 -, Cu2 +, Fe3 +, Co2 + and Ni2 +, were investigated, which suggests that their suppression to the PCVG of lead was in the order of Cl- < SO42 - < NO3- for anions and Ni2 +, Co2 + < Fe3 + < Cu2 + for transition metal ions. Under optimized conditions, relative standard derivation (RSD) of 4.4% was achieved from replicate measurements (n = 5) of a standard solution of 0.1 μg L- 1 lead. And, the limit of quantitation (LOQ, 10σ) of 0.012 μg L- 1 lead was obtained using this method and the method blank could be easily controlled down to 0.023 μg L- 1. To validate applicability of this method, it was also employed for the determination of lead in tap water, rain water and lake water.

  8. Decision Threshold and Detection Limit in Spectrometric Measurements. Part 1: Application to Gamma Spectrometry

    International Nuclear Information System (INIS)

    This report summarised the author's lecture of the advanced gamma spectrometry course organised by CIEMAT. The characteristic limits determination in gamma spectrometry generally is obtained through the programming that the trade marks offers to the client with the objective of the automatic calculation of the activity concentrations existing in a sample. In this report, the examples shown in the ISO 11929 standard are compared to the programming realised by Genie 2k for determining characteristic limits. The main difference of both is located in the uncertainty calculations due to the efficiency calibration that is considered by ISO and not by Genie 2K. Through implementation in the software developed by trade marks will be possible to introduce this uncertainty and to assimilate to the calculation done by ISO 11929. In the second part of this report will be analyzed the more complicated samples of this application as counting in a whole body counter (following ISO-28218 about Performance Criteria for radio bioassay), multiplet, overlapping, addition of several peaks for obtaining the activity concentration, etc. (Author) 19 refs.

  9. Electrochemical oxidation and cleavage of peptides analyzed with on-line mass spectrometric detection

    NARCIS (Netherlands)

    Permentier, H.P.; Jurva, U; Barroso, B.; Bruins, A.P.

    2003-01-01

    An on-line electrochernistry/electrospray mass spectrometry system (EC/MS) is described that allows fast analysis of the oxidation products of peptides. A range of peptides was oxidized in an electrochemical cell by application of a potential ramp from 0 to 1.5 V during passage of the sample. Electr

  10. On-chip electro membrane extraction with online ultraviolet and mass spectrometric detection

    DEFF Research Database (Denmark)

    Petersen, Nickolaj Jacob; Foss, Sunniva Taule; Jensen, Henrik;

    2011-01-01

    Electro membrane extraction was demonstrated in a microfluidic device. The device was composed of a 25 μm thick porous polypropylene membrane bonded between two poly(methyl methacrylate) (PMMA) substrates, each having 50 μm deep channel structures facing the membrane. The supported liquid membrane...... (SLM) consisted of 2-nitrophenyl octyl ether (NPOE) immobilized in the pores of the membrane. The driving force for the extraction was a 15 V direct current (DC) electrical potential applied across the SLM. Samples containing the basic drugs pethidine, nortriptyline, methadone, haloperidol, loperamide......L/min, enrichment factors exceeding 75 were obtained during 12 min of operation from a total sample volume of only 108 μL. The on-chip electro membrane system was coupled online to electrospray ionization mass spectrometry and used to monitor online and real-time metabolism of amitriptyline by rat liver microsomes...

  11. Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

    OpenAIRE

    Svetlana Hrouzková; Eva Matisová

    2012-01-01

    Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC) and fast CG...

  12. Mass spectrometrical detection of 81Kr in meteorites and the terrestrial age of antarctic eucrites

    International Nuclear Information System (INIS)

    From the terrestrial ages of the meteorites found at the Allan Hills in the Antarctica conditions can be derived for a possible collecting-mechanism for meteorites. Observations agree with the following model: Among the direct impact of meteorites into the area additional meteorites of a teritory about five times greater are collected by a compressive surface flow of the ice. This teritory again is provided with meteorites which are transported in the ice (maximal time for transport in ice: about 270.000 years). By ablation these meteorites reach the surface again and weathering begins. The 'half Life' for the weathering of a stone meteorite at the surface of the ice under antarctical conditions is about 110.000 years. (WB)

  13. Molecular hydrogen absorption systems in SDSS

    CERN Document Server

    Balashev, S A; Ivanchik, A V; Varshalovich, D A; Petitjean, P; Noterdaeme, P

    2014-01-01

    We present a systematic search for molecular hydrogen absorption systems at high redshift in quasar spectra from the Sloan Digital Sky Survey (SDSS) II Data Release 7 and SDSS-III Data Release 9. We have selected candidates using a modified profile fitting technique taking into account that the Ly$\\alpha$ forest can effectively mimic H$_2$ absorption systems at the resolution of SDSS data. To estimate the confidence level of the detections, we use two methods: a Monte-Carlo sampling and an analysis of control samples. The analysis of control samples allows us to define regions of the spectral quality parameter space where H$_2$ absorption systems can be confidently identified. We find that H$_2$ absorption systems with column densities $\\log {\\rm N_{H_2}} > 19$ can be detected in only less than 3% of SDSS quasar spectra. We estimate the upper limit on the detection rate of saturated H$_2$ absorption systems ($\\log {\\rm N_{H_2}} > 19$) in Damped Ly-$\\alpha$ (DLA) systems to be about 7%. We provide a sample of ...

  14. Identification of NTBC metabolites in urine from patients with hereditary tyrosinemia type 1 using two different mass spectrometric platforms: triple stage quadrupole and LTQ-Orbitrap.

    Science.gov (United States)

    Herebian, Diran; Lamshöft, Marc; Mayatepek, Ertan; Spiekerkoetter, Ute

    2010-03-01

    The objective of our work was to identify known and unknown metabolites of the drug NTBC (2-(2-nitro-4-trifluoromethylbenzoyl)-1,3-cyclohexanedione) in urine from patients during the treatment of hereditary tyrosinemia type 1 (HT-1) disease, a severe inborn error of tyrosine metabolism. Two different mass spectrometric techniques, a triple stage quadrupole and an LTQ-Orbitrap (Fourier transform mass spectrometry (FTMS)), were used for the identification and the structural elucidation of the detected metabolites. Initially, the mass spectrometric (MS) approach consisted of the precursor ion scan detection of the selected product ions, followed by the corresponding collision-induced dissociation (CID) fragmentation analysis (MS(2)) for the targeted selected reaction monitoring (SRM) mode. Subsequently, accurate and high-resolution full scan and MS/MS measurements were performed on the possible metabolites using the LTQ-Orbitrap. Final confirmation of the identified metabolites was achieved by measuring commercially supplied or laboratory-synthesized standards. Altogether six metabolites, including NTBC itself, were extracted, detected and identified. In addition, two new NTBC metabolites were unambiguously identified as amino acid conjugates, namely glycine-NTBC and beta-alanine-NTBC. These identifications were based on their characteristics of chromatographic retention times, protonated molecular ions, elemental compositions, product ions (using CID and higher-energy C-trap dissociation (HCD) techniques) and synthesized references. The applied MS strategy, based on two different MS platforms (LC/MS/MS and FTMS), allowed the rapid identification analysis of the drug metabolites from human extracts and could be used for pharmaceutical research and drug development. PMID:20187082

  15. Revisiting Absorptive Capacity

    DEFF Research Database (Denmark)

    de Araújo, Ana Luiza Lara; Ulhøi, John Parm; Lettl, Christopher

    Absorptive capacity has mostly been perceived as a 'passive' outcome of R&D investments. Recently, however, a growing interest into its 'proactive' potentials has emerged. This paper taps into this development and proposes a dynamic model for conceptualizing the determinants of the complementary...... learning processes of absorptive capacity, which comprise combinative and adaptive capabilities. Drawing on survey data (n=169), the study concludes that combinative capabilities primarily enhance transformative and exploratory learning processes, while adaptive capabilities strengthen all three learning...

  16. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide powder and pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Total Carbon by Combustion and Gravimetry 7-17 Total Boron by Titrimetry 18-28 Isotopic Composition by Mass Spectrometry 29-38 Chloride and Fluoride Separation by Pyrohydrolysis 39-45 Chloride by Constant-Current Coulometry 46-54 Fluoride by Ion-Selective Electrode 55-63 Water by Constant-Voltage Coulometry 64-72 Impurities by Spectrochemical Analysis 73-81 Soluble Boron by Titrimetry 82-95 Soluble Carbon by a Manometric Measurement 96-105 Metallic Impurities by a Direct Reader Spectrometric Method 106-114

  17. Recent developments of nanoparticle-based enrichment methods for mass spectrometric analysis in proteomics

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    In proteome research, rapid and effective separation strategies are essential for successful protein identification due to the broad dynamic range of proteins in biological samples. Some important proteins are often expressed in ultra low abundance, thus making the pre-concentration procedure before mass spectrometric analysis prerequisite. The main purpose of enrichment is to isolate target molecules from complex mixtures to reduce sample complexity and facilitate the subsequent analyzing steps. The introduction of nanoparticles into this field has accelerated the development of enrichment methods. In this review, we mainly focus on recent developments of using different nanomaterials for pre-concentration of low-abundance peptides/ proteins, including those containing post-translational modifications, such as phosphorylation and glycosylation, prior to mass spectrometric analysis.

  18. New FORTRAN computer programs to acquire and process isotopic mass-spectrometric data

    International Nuclear Information System (INIS)

    The computer programs described in New Computer Programs to Acquire and Process Isotopic Mass Spectrometric Data have been revised. This report describes in some detail the operation of these programs, which acquire and process isotopic mass spectrometric data. Both functional and overall design aspects are addressed. The three basic program units - file manipulation, data acquisition, and data processing - are discussed in turn. Step-by-step instructions are included where appropriate, and each subsection is described in enough detail to give a clear picture of its function. Organization of file structure, which is central to the entire concept, is extensively discussed with the help of numerous tables. Appendices contain flow charts and outline file structure to help a programmer unfamiliar with the programs to alter them with a minimum of lost time

  19. Integration of landsat MSS imagery with aeromagnetic and airborne spectrometric data over a part of Mozambique

    International Nuclear Information System (INIS)

    An area within the undifferentiated Precambrian gneisses and granulites of the Mozambique Belt was studied using Landsat MSS imagery, aeromagnetic data and spectrometric data. Airborne radiometric data including total count, uranium, thorium and potassium channels and aeromagnetic data were prepared as raster scanned images, which were registered and combined with the Landsat imagery on an image processing system. In addition to study of the individual data sets the spectrometric channels were manipulated to provide ratios and composite images. These composite images provided information from the three main channels, potassium, uranium and thorium. Single channel images derived from them were colour contoured and integrated with the Landsat imagery. An interpretation of the geophysical data integrated with the Landsat imagery was compared with separate interpretations of each previously carried out. The combined display techniques employed, substantially improved the discrimination of lithology within the area studied and provided a more detailed description of the regional structure. (author). 16 refs, 6 figs, 1 tab

  20. Novel concepts and strategies in anticancer metallodrug development : towards oral activity, peptide conjugation and mass spectrometric applications

    International Nuclear Information System (INIS)

    including top-down electrospray ionization-mass spectrometry (ESI-MS). Mass spectrometry is an invaluable tool in the analysis of molecular interactions between metallodrugs and biomolecules, such as DNA or proteins and their constituents. Furthermore, the molecular reactivity may give insight into the mode of action of a particular metallodrug or family of metallodrugs. Within the frame of this Ph.D. thesis, mass spectrometric techniques have been used to characterize the reactivity of representative (thio)pyr(id)onato RuII–p-cymene metallodrugs towards amino acids, nucleotides and proteins and an inverse correlation was found between extent of protein binding and antiproliferative activity, at least for these families of metallodrugs. Furthermore, the analysis of metallation sites of metallodrugs on proteins by mass spectrometric methods poses significant challenges in many cases due to low adduct detection efficiencies. Top-down mass spectrometric analysis is a promising approach to determine oxaliplatin binding sites on ubiquitin and different fragmentation techniques were investigated with the combination of higher energy C-trap dissociation (HCD) and electron transfer dissociation (ETD) tandem mass spectrometry yielding the highest information content. This approach led to the confirmation of methionine-1 as the primary and histidine-68 as the secondary binding site. (author)

  1. Mass spectrometric analysis of integral membrane proteins: application to complete mapping of bacteriorhodopsins and rhodopsin.

    OpenAIRE

    Ball, L. E.; Oatis, J. E.; Dharmasiri, K.; Busman, M.; Wang, J.; Cowden, L. B.; Galijatovic, A.; N. Chen; Crouch, R K; Knapp, D R

    1998-01-01

    Integral membrane proteins have not been readily amenable to the general methods developed for mass spectrometric (or internal Edman degradation) analysis of soluble proteins. We present here a sample preparation method and high performance liquid chromatography (HPLC) separation system which permits online HPLC-electrospray ionization mass spectrometry (ESI-MS) and -tandem mass spectrometry (MS/MS) analysis of cyanogen bromide cleavage fragments of integral membrane proteins. This method has...

  2. Mass spectrometric analysis of isotope effects in bioconversion of benzene to cyclohexanone

    Science.gov (United States)

    Nam, In-Hyun; Murugesan, Kumarasamy; Kim, Young-Mo; Yang, In-Hee; Chang, Yoon-Seok

    2006-06-01

    Pseudomonas veronii strain PH-03 has been shown to convert benzene to cyclohexanone through phenol. Mass spectrometry results revealed that unusual isotopic effects have been occurred in the transformation product, cyclohexanone. The isotopic composition was strongly depends on the compound specific hydrogen or oxygen source. The exchange of labile deuterium atoms has been investigated through electrospray ionization liquid chromatography mass spectrometry. The mass spectrometric analysis of biotransformation products enabled the proposal of a corresponding bioconversion pathway.

  3. Mass spectrometric analysis of the volatiles released by heating or crushing rocks

    Science.gov (United States)

    Barker, C.; Sommer, M. A.

    1973-01-01

    Vacuum extraction with subsequent mass spectrometric analysis of evolved volatiles was selected as the analytical procedure. The high-vacuum gas-handling system was constructed of stainless steel. The system was completely free from mercury, grease, or volatile organic materials. The furnace for heating the samples is discussed together with the high-vacuum crusher, the mass spectrometer, and approaches for water determination. The analytical procedure is considered, giving attention to the extraction of volatiles, adsorption studies, and the analysis of volatiles.

  4. Standard methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets

    International Nuclear Information System (INIS)

    Various methods are described in detail as to procedure, interferences, and limits of detection or applicability for the determination of Pu and various impurities in PuO2 powders and pellets. Methods for the determination of Pu are controlled-potential coulometry, ceric sulfate titration, and amperometric titration with Fe2+. Spectrophotometric methods are given for N and S, and a direct combustion-thermal conductivity method for the determination of total C is described. A pyrohydrolysis method is described for the determination of μg amounts of Cl- and F-. A mass spectrometric determination of the Pu isotopic content of the oxide is included, and general chemical methods are included for the determination of moisture in both powders and pellets and for total gas--exclusive of moisture--in pellets. Spectrochemical methods are described for the determination of rare earths, 36 trace elements whose recommended analytical spectral lines and concentration ranges are tabulated, and impurities occurring in the atom-ppB range

  5. Combining Mass Spectrometric Metabolic Profiling with Genomic Analysis: A Powerful Approach for Discovering Natural Products from Cyanobacteria.

    Science.gov (United States)

    Kleigrewe, Karin; Almaliti, Jehad; Tian, Isaac Yuheng; Kinnel, Robin B; Korobeynikov, Anton; Monroe, Emily A; Duggan, Brendan M; Di Marzo, Vincenzo; Sherman, David H; Dorrestein, Pieter C; Gerwick, Lena; Gerwick, William H

    2015-07-24

    An innovative approach was developed for the discovery of new natural products by combining mass spectrometric metabolic profiling with genomic analysis and resulted in the discovery of the columbamides, a new class of di- and trichlorinated acyl amides with cannabinomimetic activity. Three species of cultured marine cyanobacteria, Moorea producens 3L, Moorea producens JHB, and Moorea bouillonii PNG, were subjected to genome sequencing and analysis for their recognizable biosynthetic pathways, and this information was then compared with their respective metabolomes as detected by MS profiling. By genome analysis, a presumed regulatory domain was identified upstream of several previously described biosynthetic gene clusters in two of these cyanobacteria, M. producens 3L and M. producens JHB. A similar regulatory domain was identified in the M. bouillonii PNG genome, and a corresponding downstream biosynthetic gene cluster was located and carefully analyzed. Subsequently, MS-based molecular networking identified a series of candidate products, and these were isolated and their structures rigorously established. On the basis of their distinctive acyl amide structure, the most prevalent metabolite was evaluated for cannabinomimetic properties and found to be moderate affinity ligands for CB1.

  6. Product Identification and Mass Spectrometric Analysis of n-Butane and i-Butane Pyrolysis at Low Pressure

    Institute of Scientific and Technical Information of China (English)

    Yi-jun Zhang; Wen-hao Yuan; Jiang-huai Cai; Li-dong Zhang; Fei Qi; Yu-yang Li

    2013-01-01

    The pyrolysis of n-butane andi-butane at low pressure was investigated from 823-1823 K in an electrically heated flow reactor using synchrotron vacuum ultraviolet photoionization mass spectrometry.More than 20 species,especially several radicals and isomers,were detected and identified from the measurements of photoionization efficiency (PIE) spectra.Based on the mass spectrometric analysis,the characteristics of n-butane and i-butane pyrolysis were discussed,which provided experimental evidences for the discussion of decomposition pathways of butane isomers.It is concluded that the isomeric structures of n-butane and i-butane have strong influence on their main decomposition pathways,and lead to dramatic differences in their mass spectra and PIE spectra such as the different dominant products and isomeric structures of butene products.Furthermore,compared with n-butane,i-butane can produce strong signals of benzene at low temperature in its pyrolysis due to the enhanced formation of benzene precursors like propargyl and C4 species,which provides experimental clues to explain the higher sooting tendencies of iso-alkanes than n-alkanes.

  7. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1999-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets to determine compliance with specifications. 1.2 This test method covers the determination of uranium and the oxygen to uranium atomic ratio in nuclear-grade uranium dioxide powder and pellets. 1.4 This test method covers the determination of chlorine and fluorine in nuclear-grade uranium dioxide. With a 1 to 10-g sample, concentrations of 5 to 200 g/g of chlorine and 1 to 200 μg/g of fluorine are determined without interference. 1.5 This test method covers the determination of moisture in uranium dioxide samples. Detection limits are as low as 10 μg. 1.6 This test method covers the determination of nitride nitrogen in uranium dioxide in the range from 10 to 250 μg. 1.7 This test method covers the spectrographic analysis of nuclear-grade UO2 for the 26 elements in the ranges indicated in Table 2. 1.8 For simultaneous determination of trace ele...

  8. Development of an automated sequential injection on-line solvent extraction-back extraction procedure as demonstrated for the determination of cadmium with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2002-01-01

    An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium...

  9. Mass Spectrometric Monitoring of Animal Feed for BSE Spread

    Science.gov (United States)

    King, Angela G.

    2004-01-01

    The researchers in London have developed an emerging technology that utilizes mass spectrometry to detect processed animal protein (PAP) in animal feed. The amount of animal protein in the feed can be determined by the ratio of the hydrolyzed gelatine signal at m/z 1044 to an internal standard signal at m/z 556.

  10. Demonstration of differential backscatter absorption gas imaging

    International Nuclear Information System (INIS)

    Backscatter absorption gas imaging (BAGI) is a technique that uses infrared active imaging to generate real-time video imagery of gas plumes. We describe a method that employs imaging at two wavelengths (absorbed and not absorbed by the gas to be detected) to allow wavelength-differential BAGI. From the frames collected at each wavelength, an absorbance image is created that displays the differential absorbance of the atmosphere between the imager and the backscatter surface. This is analogous to a two-dimensional topographic differential absorption lidar or differential optical absorption spectroscopy measurement. Gas plumes are displayed, but the topographic scene image is removed. This allows a more effective display of the plume image, thus ensuring detection under a wide variety of conditions. The instrument used to generate differential BAGI is described. Data generated by the instrument are presented and analyzed to estimate sensitivity. (c) 2000 Optical Society of America

  11. Seven-effect absorption refrigeration

    Science.gov (United States)

    DeVault, Robert C.; Biermann, Wendell J.

    1989-01-01

    A seven-effect absorption refrigeration cycle is disclosed utilizing three absorption circuits. In addition, a heat exchanger is used for heating the generator of the low absorption circuit with heat rejected from the condenser and absorber of the medium absorption circuit. A heat exchanger is also provided for heating the generator of the medium absorption circuit with heat rejected from the condenser and absorber of the high absorption circuit. If desired, another heat exchanger can also be provided for heating the evaporator of the high absorption circuit with rejected heat from either the condenser or absorber of the low absorption circuit.

  12. Sphinx 1: Spectrometric photon counting and integration pixel for X-Ray imaging with a 100 electron LSB

    International Nuclear Information System (INIS)

    Sphinx1 is a novel pixel architecture adapted for X-ray imaging that can detect radiation by photon counting and by charge integration. In photon counting mode, each photon is compensated by one or more counter-charge packets which can be dimensioned at a level as low as 100 electrons and the number of injected counter-charge packets indicates the incoming photon energy, thus allowing a spectrometric detection. The pixel is also able to detect radiation by integrating the charges deposited by all incoming photons and converting this analog value into a digital data with a least significant bit (LSB) of 100 electrons through the use of the counter-charge concept. In this paper, Sphinx1 pixel architecture is presented with emphasis on the counter-charge design, and the two modes of operation are described in detail. The pixel was simulated using Eldo simulator. Simulation results indicate an equivalent noise charge (ENC) of 48 electrons-rms for a detector capacitance of 75 fF. The LSB linearity and the ENC are further studied for different values of detector capacitances. The analog and digital power consumptions are calculated to be less than 1μW in static conditions, proving the architecture to be suitable for large area detectors. Finally, corner simulations show a consistent performance against transistors mismatch. Proof of concept test chip of 5 mm * 5 mm test chip is being designed fabricated in CMOS 0.13 μm technology, with a pixel pitch of 200 μm. (authors)

  13. The Application of Atomic Absorption Spectrometry in Automatic Transmission Fault Detection%原子吸收光谱法在汽车自动变速器故障检测中的应用

    Institute of Scientific and Technical Information of China (English)

    陈立旦; 陈开考

    2012-01-01

    The authors studied the innovative applications of atomic absorption spectrometry in the automatic transmission fault detectioa After the authors have determined Fe, Cu and Cr contents in the five groups of Audi A6 main metal in automatic transmission fluid whose travel course is respectively 10~15 thousand kilometers, 20~26 thousand kilometers, 32~38 thousand kilometers, 43~49 thousand kilometers, and 52~58 thousand kilometers by atomic absorption spectrometry, the authors founded the database of primary metal content in the Audi A6 different mileage automatic transmission fluid (ATF). The research discovered that the main metal content in the automatic transmission fluid increased with the vehicles mileage and its normal metal content level in the automatic transmission fluid is between the two trend lines. The authors determined the main metal content of automatic transmission fluid which had faulty symptoms and compared it with its database value. Those can not only judge the wear condition of the automatic transmission which had faulty symptoms but also help the automobile detection and maintenance personnel to diagnose automatic transmission failure reasons without disintegration. This reduced automobile maintenance costs, and improved the quality of automobile maintenance.%研究原子吸收光谱法在汽车自动变速器故障检测中的创新性应用.通过原子吸收光谱法测定行驶里程分别为10 000~15 000,20 000~26 000,32 000~38 000,43 000~49 000,52 000~58 000km五批奥迪A6自动变速器油液(ATF)中主要金属Fe,Cu,Cr的含量,建立奥迪A6自动变速器不同行驶里程数ATF主要金属含量的数据库.研究发现主要金属含量随着汽车行驶里程数上升而增加,并且其正常含量在两条趋势线之间.测定有故障症状的ATF主要金属含量,并与其数据库数值比对,既可以判断自动变速器的磨损状况,也可以帮助汽车检测维修人员在不解体状态下诊断汽车

  14. A new ultrasonic-assisted cloud-point-extraction procedure for pre-concentration and determination of ultra-trace levels of copper in selected beverages and foods by flame atomic absorption spectrometry.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan; Orhan, Ulaş

    2015-01-01

    A new ultrasonic-assisted cloud-point-extraction (UA-CPE) method was developed for the pre-concentration of Cu(II) in selected beverage and food samples prior to flame atomic absorption spectrometric (FAAS) analysis. For this purpose, Safranin T was used as an ion-pairing reagent based on charge transfer in the presence of oxalate as the primary chelating agent at pH 10. Non-ionic surfactant, poly(ethyleneglycol-mono-p-nonylphenylether) (PONPE 7.5) was used as an extracting agent in the presence of NH4Cl as the salting out agent. The variables affecting UA-CPE efficiency were optimised in detail. The linear range for Cu(II) at pH 10 was 0.02-70 µg l(-)(1) with a very low detection limit of 6.10 ng l(-)(1), while the linear range for Cu(I) at pH 8.5 was 0.08-125 µg l(-)(1) with a detection limit of 24.4 ng l(-)(1). The relative standard deviation (RSD %) was in the range of 2.15-4.80% (n = 5). The method was successfully applied to the quantification of Cu(II), Cu(I) and total Cu in selected beverage and food samples. The accuracy of the developed method was demonstrated by the analysis of two standard reference materials (SRMs) as well as recoveries of spiked samples.

  15. Central cooling: absorptive chillers

    Energy Technology Data Exchange (ETDEWEB)

    Christian, J.E.

    1977-08-01

    This technology evaluation covers commercially available single-effect, lithium-bromide absorption chillers ranging in nominal cooling capacities of 3 to 1,660 tons and double-effect lithium-bromide chillers from 385 to 1,060 tons. The nominal COP measured at operating conditions of 12 psig input steam for the single-effect machine, 85/sup 0/ entering condenser water, and 44/sup 0/F exiting chilled-water, ranges from 0.6 to 0.65. The nominal COP for the double-effect machine varies from 1.0 to 1.15 with 144 psig entering steam. Data are provided to estimate absorption-chiller performance at off-nominal operating conditions. The part-load performance curves along with cost estimating functions help the system design engineer select absorption equipment for a particular application based on life-cycle costs. Several suggestions are offered which may be useful for interfacing an absorption chiller with the remaining Integrated Community Energy System. The ammonia-water absorption chillers are not considered to be readily available technology for ICES application; therefore, performance and cost data on them are not included in this evaluation.

  16. Peat as a natural solid-phase for copper preconcentration and determination in a multicommuted flow system coupled to flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gonzales, A.P.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Firmino, M.A. [Departamento de Engenharia de Materiais, Escola de Engenharia, Universidade Presbiteriana Mackenzie, Rua da Consolacao, 930, 01302-970 Sao Paulo (Brazil); Nomura, C.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Rocha, F.R.P.; Oliveira, P.V. [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 748, 05508-000 Sao Paulo (Brazil); Gaubeur, I. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil)], E-mail: ivanise.gaubeur@ufabc.edu.br

    2009-03-23

    The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 mol L{sup -1} HNO{sub 3}. The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 {mu}g L{sup -1}, with a detection limit estimated as 3 {mu}g L{sup -1} at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n = 20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level.

  17. Percutaneous absorption from soil.

    Science.gov (United States)

    Andersen, Rosa Marie; Coman, Garrett; Blickenstaff, Nicholas R; Maibach, Howard I

    2014-01-01

    Abstract Some natural sites, as a result of contaminants emitted into the air and subsequently deposited in soil or accidental industrial release, have high levels of organic and non-organic chemicals in soil. In occupational and recreation settings, these could be potential sources of percutaneous exposure to humans. When investigating percutaneous absorption from soil - in vitro or vivo - soil load, particle size, layering, soil "age" time, along with the methods of performing the experiment and analyzing the results must be taken into consideration. Skin absorption from soil is generally reduced compared with uptake from water/acetone. However, the absorption of some compounds, e.g., pentachlorophenol, chlorodane and PCB 1254, are similar. Lipophilic compounds like dichlorodiphenyltrichloroethane, benzo[A]pyrene, and metals have the tendency to form reservoirs in skin. Thus, one should take caution in interpreting results directly from in vitro studies for risk assessment; in vivo validations are often required for the most relevant risk assessment. PMID:25205703

  18. Mass spectrometric measurements of the isotopic anatomies of molecules (Invited)

    Science.gov (United States)

    Eiler, J. M.; Krumwiede, D.; Schlueter, H.

    2013-12-01

    Site-specific and multiple isotopic substitutions in molecular structures potentially provide an extraordinarily rich set of constraints on their sources, conditions of formation, reaction and transport histories, and perhaps other issues. Examples include carbonate ';clumped isotope' thermometry, clumped isotope measurements of CO2, O2, and, recently, methane, ethane and N2O; site-specific 15N measurements in N2O and 13C and D analyses of fatty acids, sugars, cellulose, food products, and, recently, n-alkanes. Extension of the principles behind these tools to the very large number of isotopologues of complex molecules could potentially lead to new uses of isotope chemistry, similar to proteomics, metabolomics and genomics in their complexity and depth of detail (';isotomics'?). Several technologies are potentially useful for this field, including ';SNIF-NMR', gas source mass spectrometry and IR absorption spectroscopy. However, all well established methods have restrictive limits in the sizes of samples, types of analyzes, and the sorts of isotopologues that can be measured with useful precision. We will present an overview of several emerging instruments and techniques of high-resolution gas source mass spectrometry that may enable study of a large proportion of the isotopologues of a wide range of volatile and semi-volatile compounds, including many organics, with precisions and sample sizes suitable for a range of applications. A variety of isotopologues can be measured by combining information from the Thermo 253 Ultra (a new high resolution, multi-collector gas source mass spectrometer) and the Thermo DFS (a very high resolution single collector, but used here on a novel mode to achieve ~per mil precision ratio measurements), sometimes supplemented by conventional bulk isotopic measurements. It is possible to design methods in which no one of these sources of data meaningfully constrain abundances of specific isotopologues, but their combination fully and

  19. Yafet-Kittel-type magnetic ordering in Ni{sub 0.35}Zn{sub 0.65}Fe{sub 2}O{sub 4} ferrite detected by magnetosensitive microwave absorption measurements

    Energy Technology Data Exchange (ETDEWEB)

    Alvarez, G., E-mail: memodin@yahoo.co [Departamento de Materiales Metalicos y Ceramicos, Instituto de Investigaciones en Materiales, Universidad Nacional Autonoma de Mexico, Apartado Postal 70-360, Coyoacan, DF 04510 Mexico (Mexico); Montiel, H.; Barron, J.F. [Departamento de Tecnociencias, Centro de Ciencias Aplicadas y Desarrollo Tecnologico de la Universidad Nacional Autonoma de Mexico, Mexico, DF 04510 (Mexico); Gutierrez, M.P. [Universidad Anahuac, Mexico Norte, Mexico DF (Mexico); Zamorano, R. [Departamento de Fisica, ESFM-IPN, U. P. Adolfo Lopez Mateos Edificio 9, Av. Instituto Politecnico Nacional S/N, Col. San Pedro Zacatenco, 07738 DF (Mexico)

    2010-02-15

    Magnetosensitive microwave absorption measurements of polycrystalline ferrite Ni{sub 0.35}Zn{sub 0.65}Fe{sub 2}O{sub 4} was carried out at 9.4 GHz (X-band) as a function of temperature. Temperature dependence of the total linewidth (DELTAH{sub pp}) deduced from the resonance spectra showed the passage through the Curie point (T{sub c}approx430 K). Additionally, the plot DELTAH{sub pp} vs. T also indicated the existence of another magnetic phase transition at approx240 K, which can be associated with a Yafet-Kittel-type canting of the magnetic moments. Low-field microwave absorption (LFMA) and the magnetically modulated microwave absorption spectroscopy (MAMMAS) were used to give a further knowledge on this material. For low temperature, these techniques give evidence of a Yafet-Kittel-type canting of the magnetic moments.

  20. Chemical Absorption Materials

    DEFF Research Database (Denmark)

    Thomsen, Kaj

    2011-01-01

    Chemical absorption materials that potentially can be used for post combustion carbon dioxide capture are discussed. They fall into five groups, alkanolamines, alkali carbonates, ammonia, amino acid salts, and ionic liquids. The chemistry of the materials is discussed and advantages and drawbacks...

  1. Absorption driven focus shift

    Science.gov (United States)

    Harrop, N.; Wolf, S.; Maerten, O.; Dudek, K.; Ballach, S.; Kramer, R.

    2016-03-01

    Modern high brilliance near infrared lasers have seen a tremendous growth in applications throughout the world. Increased productivity has been achieved by higher laser power and increased brilliance of lasers. Positive impacts on the performance and costs of parts are opposed to threats on process stability and quality, namely shift of focus position over time. A high initial process quality will be reduced by contamination of optics, eventually leading to a focus shift or even destruction of the optics. Focus analysis at full power of multi-kilowatt high brilliance lasers is a very demanding task because of high power densities in the spot and the high power load on optical elements. With the newly developed high power projection optics, the High-Power Micro-Spot Monitor High Brilliance (HP-MSM-HB) is able to measure focus diameter as low as 20 μm at power levels up to 10 kW at very low internal focus shift. A main driving factor behind thermally induced focus shift is the absorption level of the optical element. A newly developed measuring system is designed to determine the relative absorption level in reference to a gold standard. Test results presented show a direct correlation between absorption levels and focus shift. The ability to determine the absorption level of optical elements as well as their performance at full processing power before they are put to use, enables a high level of quality assurance for optics manufacturers and processing head manufacturers alike.

  2. ZINC ABSORPTION BY INFANTS

    Science.gov (United States)

    Zinc is a vital mineral in human nutrition, and rare cases of overt zinc deficiency are well described in term and preterm infants. A variety of methods have been developed to assess zinc absorption, retention, and balance in humans, either using mass (metabolic) balance or stable isotope-based METH...

  3. NOVEL SPECTRUM ABSORPTION OPTICAL FIBER METHANE SENSOR

    Institute of Scientific and Technical Information of China (English)

    Wang Shutao; Che Rensheng

    2005-01-01

    Based on spectrum principle and analyzing the infrared absorption spectrum of methane, a kind of optical fiber methane gas sensor and its system are developed. DFBLD(Distributed feedback laser diode) in 1 300 nm waveband is used as illuminant and phase-detecting technology is used to carry out harmonic wave detecting the concentration of methane. The sensitivity can arrive at 10-5.Experiments results show that the performance targets of the sensor such as sensitivity can basically satisfy the requests of methane detection.

  4. Three-dimensional interferometric, spectrometric, and planetary views of Procyon

    CERN Document Server

    Chiavassa, A; Kervella, P; Matter, A; Lopez, B; Collet, R; Magic, Z; Asplund, M

    2012-01-01

    We used a new realistic 3D radiative-hydrodynamical model atmosphere of Procyon generated with the Stagger Code and synthetic spectra computed with the radiative transfer code Optim3D to re-analyze interferometric and spectroscopic data from the optical to the infrared of Procyon. We compute intensity maps in two optical filters centered at 500 and 800 nm (MARK III) and one infrared filter centered at 2200 nm (VINCI). We constructed stellar disk images accounting for the center-to-limb variations and used them to derive visibility amplitudes and closure phases. We provide 3D limb-darkening coefficients in the optical as well as in the infrared. We show that visibility curves and closure phases show clear deviations from circular symmetry from the 3rd lobe on. These deviations are detectable with current interferometers using closure phases. We derive new angular diameters at different wavelengths with two independent methods based on 3D simulations. We find a diameter_Vinci = 5.390 \\pm 0.03 mas that this is c...

  5. Absorption and fluorescence spectroscopy on a smartphone

    Science.gov (United States)

    Hossain, Md. Arafat; Canning, John; Cook, Kevin; Ast, Sandra; Rutledge, Peter J.; Jamalipour, Abbas

    2015-07-01

    A self-powered smartphone-based field-portable "dual" spectrometer has been developed for both absorption and fluorescence measurements. The smartphone's existing flash LED has sufficient optical irradiance to undertake absorption measurements within a 3D-printed case containing a low cost nano-imprinted polymer diffraction grating. A UV (λex ~ 370 nm) and VIS (λex ~ 450 nm) LED are wired into the circuit of the flash LED to provide an excitation source for fluorescence measurements. Using a customized app on the smartphone, measurements of absorption and fluorescence spectra are demonstrated using pH-sensitive and Zn2+-responsive probes. Detection over a 300 nm span with 0.42 nm/pixel spectral resolution is demonstrated. Despite the low cost and small size of the portable spectrometer, the results compare well with bench top instruments.

  6. Performance analysis of gamma ray spectrometric parameters on digital signal and analog signal processing based MCA systems using NaI(Tl) detector

    Energy Technology Data Exchange (ETDEWEB)

    Kukreti, B.M., E-mail: bharatkuk@gmail.com [Atomic Minerals Directorate for Exploration and Research, Physics Laboratory, Department of Atomic Energy, Nongmynsong, AMD Complex, Shillong, Meghalaya 793019 (India); Sharma, G.K. [Atomic Minerals Directorate for Exploration and Research, Physics Laboratory, Department of Atomic Energy, Nongmynsong, AMD Complex, Shillong, Meghalaya 793019 (India)

    2012-05-15

    Accurate and speedy estimations of ppm range uranium and thorium in the geological and rock samples are most useful towards ongoing uranium investigations and identification of favorable radioactive zones in the exploration field areas. In this study with the existing 5 in. Multiplication-Sign 4 in. NaI(Tl) detector setup, prevailing background and time constraints, an enhanced geometrical setup has been worked out to improve the minimum detection limits for primordial radioelements K{sup 40}, U{sup 238} and Th{sup 232}. This geometrical setup has been integrated with the newly introduced, digital signal processing based MCA system for the routine spectrometric analysis of low concentration rock samples. Stability performance, during the long counting hours, for digital signal processing MCA system and its predecessor NIM bin based MCA system has been monitored, using the concept of statistical process control. Monitored results, over a time span of few months, have been quantified in terms of spectrometer's parameters such as Compton striping constants and Channel sensitivities, used for evaluating primordial radio element concentrations (K{sup 40}, U{sup 238} and Th{sup 232}) in geological samples. Results indicate stable dMCA performance, with a tendency of higher relative variance, about mean, particularly for Compton stripping constants. - Highlights: Black-Right-Pointing-Pointer Geometrical enhancement for ppm range primordial radio elemental determination. Black-Right-Pointing-Pointer Experimental constraints include detector setup, background and counting time. Black-Right-Pointing-Pointer Gamma spectrometric performance monitored on digital and analog MCA systems. Black-Right-Pointing-Pointer Study indicates higher variance of Compton stripping constants on digital MCA system.

  7. Ultraschall-Geschwindigkeit und-Absorption in Bi-In-Schmelzen /Ultrasonic Velocity and Absorption in Bi-In-melts

    Science.gov (United States)

    Bek, R.; Steeb, S.

    1981-02-01

    Using the pulse-echo method the ultrasonic velocity and absorption was measured with Bi-In-melts in the temperature range from liquidus up to more than 600 °C. The frequencies used reached from 10 MHz up to 130 MHz. Within the experimental accuracy no frequency dependence of the absorption coefficient α/f2 could be detected. An excess absorption can be observed, which for the molten elements can be explained by fluctuations of the packing density. For the molten alloys additionally concentration fluctuations play an important role. Thus an understanding of the temperature dependency of the ultrasonic velocity and absorption can be achieved.

  8. Mass spectrometric methods for the direct elemental and isotopic analysis of solid material

    Science.gov (United States)

    Ganeev, A. A.; Gubal, A. R.; Potapov, S. V.; Agafonova, N. N.; Nemets, V. M.

    2016-04-01

    Methods for the direct analysis of solids have a number of undeniable advantages over the methods that require preliminary dissolution of samples. High sensitivity and selectivity make the direct mass spectrometric techniques the most in-demand. The review concerns spark source mass spectrometry, laser ionization mass spectrometry, laser ablation inductively coupled plasma mass spectrometry, secondary ion mass spectrometry, secondary neutral mass spectrometry and glow discharge mass spectrometry. Basic principles, analytical characteristics and trends in the development of these techniques are discussed. Particular attention is given to applications of the techniques as well as to their competitive advantages and drawbacks. The bibliography includes 123 references.

  9. Mass spectrometric studies on irradiated (U, Pu) mixed carbide fuel of Fbtr

    Energy Technology Data Exchange (ETDEWEB)

    Balasubramanian, R. [Fuel Chemistry Division, IGCAR, Kalpakkam 603 102, Tamil Nadu (India)]. E-mail: rbs@igcar.ernet.in; Darwin Albert Raj, D.; Nalini, S.; Sai Baba, M. [Fuel Chemistry Division, IGCAR, Kalpakkam 603 102, Tamil Nadu (India)

    2005-07-01

    Mass spectrometry was employed to characterise the irradiated mixed carbide fuel of fast breeder test reactor (FBTR) for assessing its performance: thermal ionisation mass spectrometry to determine the isotopic composition, concentrations of U, Pu and Nd in the dissolver solutions and to deduce the burn-up, and a quadrupole mass spectrometric system to obtain the percentage release of fission gases (Kr + Xe). A summary and analysis of the results obtained with the fuel at 25,000 and 50,000 MWd/t in these studies is given in this paper. (author)

  10. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide

    Energy Technology Data Exchange (ETDEWEB)

    1981-01-01

    The standard covers analytical procedures to determine compliance of nuclear-grade boron carbide powder and pellets to specifications. The following methods are described in detail: total carbon by combustion and gravimetry; total boron by titrimetry; isotopic composition by mass spectrometry; chloride and fluoride separation by pyrohydrolysis; chloride by constant-current coulometry; fluoride by ion-selective electrode; water by constant-voltage coulometry; impurities by spectrochemical analysis; soluble boron by titrimetry; soluble carbon by a manometric measurement; metallic impurities by a direct reader spectrometric method. (JMT)

  11. 用于测量亚硝酸的长光程吸收光谱仪的研制%Development of a Home-Made Long Path Absorption Photometer for the Sensitive Detection of Nitrous Acid

    Institute of Scientific and Technical Information of China (English)

    陈林; 侯思齐; 王炜罡; 佟胜睿; 裴克梅; 葛茂发

    2014-01-01

    基于湿化学采样及光学检测的方法,自行搭建了长光程吸收光谱仪(LOPAP)用于检测痕量的亚硝酸.该仪器成本低,响应时间快,灵敏度高,检测限低,可以连续测量并且排除了现有其他仪器存在干扰影响的问题,既能够对大气中的痕量亚硝酸进行测量,又能检测例如烟雾箱和废气中高浓度的亚硝酸.该仪器采用双通道系统,通过将两个通道测量信号相减可以减小测量中未知干扰物的影响.仪器的检测限可以达到9×10-12 mol∙mol-1,响应时间为5 min,其准确度为±10%.另外对NO、NO2、O3、NO2+O3、NO2+SO2、O3+HONO等气体进行了仪器的干扰分析,发现只有当NO2存在时才有很弱的HONO干扰信号产生,干扰值大约为0.02%.同时在2013年8月29日到9月4日对HONO在中国科学院化学研究所进行了为期六天的外场观测,分析了HONO的日浓度变化,以及这种变化与光照强度、NOx浓度和NO2浓度之间的关系. HONO/NO2的比率表明除了NO2的非均相反应外还存在未知来源.%Nitrous acid (HONO) is an important trace gas in tropospheric photochemistry, which plays a significant role in pol uted urban atmosphere. Based on the measuring principle, a long path absorption photometer (LOPAP) for the detection of nitrous acid was built in-house, which uses wet chemical sampling and photometric detection. This instrument aims to overcome the known problems with current HONO measurement techniques and was designed to be a cheap, sensitive, compact, and continuously working HONO monitor for ambient air measurements in the troposphere, or for measurements of higher concentration, e.g., in a smog chamber and in exhaust gases. The system includes two channels, by subtracting the signal of the second channel from the first channel the occurrence of possible unknown interferences can be minimized. The instrument has a detection limit of 9×10-12 mol∙mol-1 and an accuracy of 10%at 5 min resolution, with a good

  12. Absorptive Capacity and Diversity

    DEFF Research Database (Denmark)

    Kristinsson, Kári

    that contribute to the neo-Schumpeterian economics literature and hopefully inspires further research into this area. The main findings of the dissertation can be divided into four distinct parts. First, diversity of individuals within firms is associated with firm innovative performance. This is in line......One of the most influential contributions to neo-Schumpeterian economics is Cohen and Levinthal‘s papers on absorptive capacity. Since their publication in the late 1980s and early 1990s the concept absorptive capacity has had substantial impact on research in economics and management, including...... international business, organizational economics, strategic management, technology management and last but not least neo-Schumpeterian economics. The goal of this dissertation is to examine what many consider as neglected arguments from the work by Cohen and Levinthal and thereby illuminate an otherwise...

  13. X-ray absorption spectroscopy of metalloproteins.

    Science.gov (United States)

    Ward, Jesse; Ollmann, Emily; Maxey, Evan; Finney, Lydia A

    2014-01-01

    Metalloproteins are enormously important in biology. While a variety of techniques exist for studying metals in biology, X-ray absorption spectroscopy is particularly useful in that it can determine the local electronic and physical structure around the metal center, and is one of the few avenues for studying "spectroscopically silent" metal ions like Zn(II) and Cu(I) that have completely filled valence bands. While X-ray absorption near-edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) are useful for studying metalloprotein structure, they suffer the limitation that the detected signal is an average of all the various metal centers in the sample, which limits its usefulness for studying metal centers in situ or in cell lysates. It would be desirable to be able to separate the various proteins in a mixture prior to performing X-ray absorption studies, so that the derived signal is from one species only. Here we describe a method for performing X-ray absorption spectroscopy on protein bands following electrophoretic separation and western blotting.

  14. Parallel Workflow for High-Throughput (>1,000 Samples/Day) Quantitative Analysis of Human Insulin-Like Growth Factor 1 Using Mass Spectrometric Immunoassay

    Science.gov (United States)

    Oran, Paul E.; Trenchevska, Olgica; Nedelkov, Dobrin; Borges, Chad R.; Schaab, Matthew R.; Rehder, Douglas S.; Jarvis, Jason W.; Sherma, Nisha D.; Shen, Luhui; Krastins, Bryan; Lopez, Mary F.; Schwenke, Dawn C.; Reaven, Peter D.; Nelson, Randall W.

    2014-01-01

    Insulin-like growth factor 1 (IGF1) is an important biomarker for the management of growth hormone disorders. Recently there has been rising interest in deploying mass spectrometric (MS) methods of detection for measuring IGF1. However, widespread clinical adoption of any MS-based IGF1 assay will require increased throughput and speed to justify the costs of analyses, and robust industrial platforms that are reproducible across laboratories. Presented here is an MS-based quantitative IGF1 assay with performance rating of >1,000 samples/day, and a capability of quantifying IGF1 point mutations and posttranslational modifications. The throughput of the IGF1 mass spectrometric immunoassay (MSIA) benefited from a simplified sample preparation step, IGF1 immunocapture in a tip format, and high-throughput MALDI-TOF MS analysis. The Limit of Detection and Limit of Quantification of the resulting assay were 1.5 μg/L and 5 μg/L, respectively, with intra- and inter-assay precision CVs of less than 10%, and good linearity and recovery characteristics. The IGF1 MSIA was benchmarked against commercially available IGF1 ELISA via Bland-Altman method comparison test, resulting in a slight positive bias of 16%. The IGF1 MSIA was employed in an optimized parallel workflow utilizing two pipetting robots and MALDI-TOF-MS instruments synced into one-hour phases of sample preparation, extraction and MSIA pipette tip elution, MS data collection, and data processing. Using this workflow, high-throughput IGF1 quantification of 1,054 human samples was achieved in approximately 9 hours. This rate of assaying is a significant improvement over existing MS-based IGF1 assays, and is on par with that of the enzyme-based immunoassays. Furthermore, a mutation was detected in ∼1% of the samples (SNP: rs17884626, creating an A→T substitution at position 67 of the IGF1), demonstrating the capability of IGF1 MSIA to detect point mutations and posttranslational modifications. PMID:24664114

  15. Parallel workflow for high-throughput (>1,000 samples/day quantitative analysis of human insulin-like growth factor 1 using mass spectrometric immunoassay.

    Directory of Open Access Journals (Sweden)

    Paul E Oran

    Full Text Available Insulin-like growth factor 1 (IGF1 is an important biomarker for the management of growth hormone disorders. Recently there has been rising interest in deploying mass spectrometric (MS methods of detection for measuring IGF1. However, widespread clinical adoption of any MS-based IGF1 assay will require increased throughput and speed to justify the costs of analyses, and robust industrial platforms that are reproducible across laboratories. Presented here is an MS-based quantitative IGF1 assay with performance rating of >1,000 samples/day, and a capability of quantifying IGF1 point mutations and posttranslational modifications. The throughput of the IGF1 mass spectrometric immunoassay (MSIA benefited from a simplified sample preparation step, IGF1 immunocapture in a tip format, and high-throughput MALDI-TOF MS analysis. The Limit of Detection and Limit of Quantification of the resulting assay were 1.5 μg/L and 5 μg/L, respectively, with intra- and inter-assay precision CVs of less than 10%, and good linearity and recovery characteristics. The IGF1 MSIA was benchmarked against commercially available IGF1 ELISA via Bland-Altman method comparison test, resulting in a slight positive bias of 16%. The IGF1 MSIA was employed in an optimized parallel workflow utilizing two pipetting robots and MALDI-TOF-MS instruments synced into one-hour phases of sample preparation, extraction and MSIA pipette tip elution, MS data collection, and data processing. Using this workflow, high-throughput IGF1 quantification of 1,054 human samples was achieved in approximately 9 hours. This rate of assaying is a significant improvement over existing MS-based IGF1 assays, and is on par with that of the enzyme-based immunoassays. Furthermore, a mutation was detected in ∼1% of the samples (SNP: rs17884626, creating an A→T substitution at position 67 of the IGF1, demonstrating the capability of IGF1 MSIA to detect point mutations and posttranslational modifications.

  16. Determination of trace quantities of uranium in rocks mass spectrometric isotope dilution technique

    International Nuclear Information System (INIS)

    A detailed experimental investigation on the thermionic emission of uranium deposited on a single flat type rhenium filament has been carried out. The study was aimed at determining the influence of various forms of deposition on the emission sensitivity and thermal stability of U+ , UO+ and UO2+ ions. Based on these investigations, a technique, involving an addition of a small quantity of colloidal suspension of graphite on top of the uranyl nitrate sample deposited, was chosen because of its higher, emission sensitivity for uranium metal ions. The experimental parameters of the technique were optimised and the technique was employed in the determination of trace quantities of uranium in rock samples using mass spectrometric isotope dilution method. For the mass spectrometric isotope dilution analysis National Bureau of Standards uranium isotopic standard NBS-U 970 was employed as a tracer, where as the mass discrimination effect in the uranium isotope analysis was corrected using the uranium isotopic standard NBS-U500. Uranium was determined in each of the seven granite samples from Wyoming, USA and two USGS standard rocks. The precision of the analysis was found to be ±1% . The uranium values obtained on the rock samples were compared with the analyses of other investigators. Influence of the sample splitting on the uranium analysis was discussed in the light of the analytical results obtained.(author)

  17. MALDI mass spectrometric imaging meets "omics": recent advances in the fruitful marriage.

    Science.gov (United States)

    Crecelius, A C; Schubert, U S; von Eggeling, F

    2015-09-01

    Matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI MSI) is a method that allows the investigation of the molecular content of surfaces, in particular, tissues, within its morphological context. The applications of MALDI MSI in the field of large-scale mass spectrometric studies, which are typically denoted by the suffix "omics", are steadily increasing. This is because, on the one hand, technical advances regarding sample collection and preparation, matrix application, instrumentation, and data processing have enhanced the molecular specificity and sensitivity of MALDI MSI; on the other hand, the focus of the "omics" community has moved from establishing an inventory of certain compound classes to exploring their spatial distribution to gain novel insights. Thus, the aim of this mini-review is twofold, to display the state-of-the-art in terms of technical aspects in MALDI MSI and to highlight selected applications in the last two years, which either have significantly advanced a certain "omics" field or have introduced a new one through pioneering efforts. PMID:26161715

  18. New miniaturized alpha/beta spectrometric systems for the surface contamination monitoring and radon personal dosimeter

    International Nuclear Information System (INIS)

    We report on a new miniaturized alpha/beta spectrometric system. This cheque cart 12 bit SARAD spectra 5011 spectrometric system we can combine with a new developed detector, preamp and forming unit. A very important application of this new measuring system is the alpha nuclidspecific surface contamination monitoring. Especially in old nuclear power station it is very important in the decommissioning process to know the nuclide vector. We report of applications to use this new technology to measure the nuclide vector in old lead cells or construction elements in old nuclear reactors. We measure surface contamination in the order of 1 Bq/cm2 of Pu-239 very easy. A other modification of this cheque cart spectrometer is the radon personal dosimeter. In this case we have integrated on a cheque cart a 8 bit spectrometer, a 1cm2 silicon detector, the signal processing, AD-conversion, data storage and transponder system for the data transfer. Using this transponder system we can also use a local resoluted dosimetry. The main application of this system is the radon dosimetry on workplaces, for instance water works, mines, show caves and other work places with high radon levels. This easy system can replace the passive screening methods and also the nuclear track etch dosimeters. Because the low price and the easy data read out the amortisation of such a electronic system is in the order of two years

  19. Particle size independent spectrometric determination of wear metals in aircraft lubricating oils

    International Nuclear Information System (INIS)

    A method for the particle size independent determination of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti in synthetic ester lubricating oils by spectrometric analysis is presented. Partial dissolution of Cr, Si, Pb, and Ag also occurs. Used ester lubricating oils as well as samples prepared with -325 mesh (44 μm) or -200 mesh (74 μm) metal powders were reacted with a small amount of hydrofluoric acid and aqua regia at 650C for 45 min with ultrasonic agitation. The reacted mixture was then diluted with a methyl isobutyl ketone and isopropyl alcohol mixture and analyzed spectrometrically. The recoveries for metal powder suspensions of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti ranged from 97 to 103% and the relative standard deviation ranged from 4 to 10%. In addition to the metal powder suspensions, over 200 aircraft oil samples were analyzed. The method is much faster and more convenient than previously reported particle size independent methods using ashing techniques

  20. Pion absorption processes

    International Nuclear Information System (INIS)

    Proton and deuteron production from low-energy pion absorption in light nuclei leading to discrete and continuum states were measured. The LEP beam line at LAMPF was used with a stack of 8 intrinsic germanium crystals. The proton energy spectra are in general characterized by a broad bump at an energy approximately corresponding to π+d → pp reaction kinematics, suggestive of pion absorption on 2 nucleons. The energy-integrated cross-section for production of deuterons has an angular distribution similar to that for production of protons. The dependence of the total pion absorption cross-section on A is explained using a semi-classical model for pion transport in nuclei. The (π+,p) as well as (π+,d) reactions generally favor transitions involving larger angular momentum transfer to the residual nucleus when states of similar nuclear structure are considered. The low-energy excitation spectra from the (π+,p) reaction are similar to the spectra from (p,d) reaction on 12C and 13C. However, a calculation of the (π+,p) cross-section using the measured (p,d) reaction with the formulation of Wilkin to relate the two reactions is in moderate disagreement with the measured (π+,p) cross-sections. The excitation spectra from the (π+,p) reaction indicte the importance of two-step processes for the reaction. The (π+,d) reaction leading to the ground state of -- residual nucleus has been seen for 7Li, 12C, and 13C targets. The measured cross section for the 12C(π+,d)10C reaction to the 2+ state is much higher than that for the ground state. For the case of 18O, no counts were seen for excitation energy of +,d) reaction