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Sample records for atomic fluorescence spectrometric

  1. High performance liquid chromatography--atomic fluorescence spectrometric determination of arsenic species in beer samples

    Energy Technology Data Exchange (ETDEWEB)

    Melo Coelho, N.M.; Parrilla, Carmen; Cervera, M.L.; Pastor, A.; Guardia, M. de la

    2003-04-10

    A method has been developed for the direct determination of As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As(V) in beers by hydride generation--atomic fluorescence spectrometry after separation of arsenic species by high performance liquid chromatography. Compounds were separated by anion-exchange chromatography with isocratic elution using KH{sub 2}PO{sub 4}/K{sub 2}HPO{sub 4} as mobile phase with elution times of 1.67, 2.08, 6.52 and 10.72 min for As(III), DMA, MMA and As(V), respectively. Parameters affecting the hydride generation of all arsenic species were studied and the best conditions were established as a reaction coil of 150 cm, for a sample injected volume of 100 {mu}l, a 4.0% (m/v) solution of sodium tetrahydroborate and 2.0 mol l{sup -1} hydrochloric acid with flow rates of 2.7 and 1.7 ml min{sup -1}, respectively and a flow rate of 500 ml min{sup -1} for the argon carrier gas. Under the best experimental conditions, the detection limit was found to be 0.12, 0.20, 0.27 and 0.39 {mu}g l{sup -1} for As(III), DMA, MMA and As(V), respectively. The relative standard deviation for eight independent determinations varied from 3.9 till 8.9% for species considered at a concentration level of 10.0 {mu}g l{sup -1}. Recovery and comparative studies evidenced that the method is suitable for the accurate determination of arsenic species in water and beer samples.

  2. 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.

  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. [Butanol extraction combined with dilute hydrochloric acid dissolution-atomic fluorescence spectrometric method for indirect determination of molybdenum in Chinese herbal medicine].

    Science.gov (United States)

    Lu, Jian-Ping; Geng, Guo-Xing; Tang, Yan-Kui; Lu, Zhi-Yong

    2012-12-01

    A method for indirectly determining the molybdenum in Chinese herbal medicine by butanol extraction and dilute hydrochloric acid dissolution was established for atomic fluorescence spectrometry. The molybdoarsenate heteropoly acid, formed in the presence of As(V) and ammonium molybdate in 0.3 mol x L(-1) sulphuric acid medium, was separated and enriched in the organic solvent, then the evaporation of organic reagent was implemented and the left residue was dissolved in dilute hydrochloric acid in which the arsenic content was determined on behalf of molybdenum. In the optimum experimental conditions, molybdenum content in 0-15 microg x L(-1) range depicts a good linear relationship, the detection limit and relative standard deviation of 0.44 microg x L(-1) and 1.1% were obtained, respectively. Spiked Chinese herbal medicine samples were determined with the proposed method, and recoveries of 95.6%-101.3% were achieved.

  5. Ultraviolet vapor generation atomic fluorescence spectrometric determination of mercury in natural water with enrichment by on-line solid phase extraction

    Science.gov (United States)

    Qin, Deyuan; Gao, Feng; Zhang, Zhaohui; Zhao, Liqian; Liu, Jixin; Ye, Jianping; Li, Junwei; Zheng, Fengxi

    2013-10-01

    A novel method, which coupled an on-line solid phase extraction (SPE) enrichment with ultraviolet vapor generation (UVG) atomic fluorescence spectrometry (AFS), was developed to improve the sensitivity of mercury determination and to remove the interference of some anion and organics to UVG of mercury. A high mercury retention efficiency and maximum exclusion of inorganic and organic matrix in water samples were achieved by using C18 SPE mini cartridge modified with sodium diethyldithiocarbamate (DDTC). Fast and efficient elution from the cartridge was found by using L-cysteine mixing solution. Furthermore, through the investigation of different UV reactor designs, the most important factor was the structure of the reactor (which corresponded roughly to the photon flux) wherein the tubing was sintered into the UV lamp to give the highest UV generation efficiency. The second factor was the materials of the tubing (which roughly corresponded to the working wavelength). Synthetic quartz, characterized by the highest transparency at 185 nm, attained the highest UVG efficiency, suggesting that the most favorable wavelength for UVG was 185 nm. Under optimum conditions, the achievable detection limit (3σ) with sample loadings of 10.0 mL was 0.03 ng L- 1 and 0.08 ng L- 1 with different manifolds, respectively. The method was successfully applied to the determination of Hg in tap water, river water and lake water samples.

  6. [Oil atomic spectrometric feature selection by Parzen window based vague sets theory].

    Science.gov (United States)

    Xu, Chao; Zhang, Pei-Lin; Ren, Guo-Quan; Zhang, Xiao-Dong; Yang, Yu-Dong

    2011-02-01

    Large quantity and ambiguity of oil atomic spectrometric information greatly affects the applicable efficiency and accuracy in fault diagnosis. A novel method for choosing less and effective spectrometric features is presented. Based on gearbox test bed, we simulated the normal wear state and two typical faults to acquire the lubricant samples. The three wear states are regarded as three vague sets, and spectrometric feature values are vague values on vague sets. Based on similarity between vague values, mean vague sensibility (MVS) is defined to describe the sensitive degree of spectrometric feature to wear state. Besides, the membership degrees of vague sets greatly depend on human experience. The probability density distribution of spectrometric data of three wear states was estimated with Parzen window. Combined with Bayesian formula, the range of vague sets membership was calculated. Experimental results verify that the proposed method is of efficient help in choosing high fault-sensitive features from so many spectrometric features.

  7. 高压消解-原子荧光光谱法测定牛初乳中硒的研究%High Pressure Digestion - Atomic Fluorescence Spectrometric Determination of Selenium in Bovine Colostrum

    Institute of Scientific and Technical Information of China (English)

    汪波; 辛跃珍

    2012-01-01

    Established by hydride atomic fluorescence method for the determination of selenium in bovine colostrum, investigates the methods of pretreatment and atom fluorescence instrument effects on the experimental results, and finally determine the digestion reagent6: 2: : 1: nitrate hydrogen peroxide: ultrapure water, with high pressure digestion of bovine colostrum samples, digestion temperature 130-140C, time 2-3hours; atomic fluorescence reducing agent forl4g / L potassium borohydride, load flow solution for 5% hydrochloric acid. Get the selenium detection limit of0.1ng / ml, the relative standard deviation for0.!6%-1.61%, recovery rate range for 88%-102%.%建立了用氢化物原子荧光法测定牛初乳中的硒,考察了前处理方法和原子荧光仪器对实验结果的影响,最后确定了消解试剂6:2::1的硝酸:过氧化氢:超纯水,用高压消解法处理牛初乳样品,消解温度130—140℃,时间2—3小时;原子荧光的还原剂为14g/l的硼氢化钾,载流液为5%的盐酸。得到硒的检出限0.1ng/ml,相对标准偏差为0.16%-1.61%,回收率范围为88%-102%。

  8. A Spectrometric Setup for Synchronous Total Internal Reflection Fluorescence Measurement at the Solid/Liquid Interface

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A spectrometric setup to perform total internal reflection fluorescence (TIRF) and synchronous TIRF measurements at solid/liquid interfaces is presented. The combination of TIRF and synchronous fluorescence was proposed to analyze simultaneously different components at interfaces. The TIRF excitation, emission and synchronous spectra of a water-soluble porphyrin were obtained from water/glass interface using this setup without the existence of a surfactant.

  9. Imaging an atomic beam using fluorescence

    Institute of Scientific and Technical Information of China (English)

    Ming He(何明); Jin Wang(王谨); Mingsheng Zhan(詹明生)

    2003-01-01

    A fluorescence detection scheme is applied to image an atomic beam. Using two laser diodes as the sources of detection light and pumping light respectively, the fluorescence image of the atomic beam is then observed by a commercial CCD-camera, which is corresponding to the atomic state and velocity distribution. The detection scheme has a great utilization in the experiments of cold atoms and atomic optics.

  10. 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%.

  11. Mass Spectrometric Imaging of Red Fluorescent Protein in Breast Tumor Xenografts

    Science.gov (United States)

    Chughtai, Kamila; Jiang, Lu; Post, Harm; Winnard, Paul T.; Greenwood, Tiffany R.; Raman, Venu; Bhujwalla, Zaver M.; Heeren, Ron M. A.; Glunde, Kristine

    2013-05-01

    Mass spectrometric imaging (MSI) in combination with electrospray mass spectrometry (ESI-MS) is a powerful technique for visualization and identification of a variety of different biomolecules directly from thin tissue sections. As commonly used tools for molecular reporting, fluorescent proteins are molecular reporter tools that have enabled the elucidation of a multitude of biological pathways and processes. To combine these two approaches, we have performed targeted MS analysis and MALDI-MSI visualization of a tandem dimer (td)Tomato red fluorescent protein, which was expressed exclusively in the hypoxic regions of a breast tumor xenograft model. For the first time, a fluorescent protein has been visualized by both optical microscopy and MALDI-MSI. Visualization of tdTomato by MALDI-MSI directly from breast tumor tissue sections will allow us to simultaneously detect and subsequently identify novel molecules present in hypoxic regions of the tumor. MS and MALDI-MSI of fluorescent proteins, as exemplified in our study, is useful for studies in which the advantages of MS and MSI will benefit from the combination with molecular approaches that use fluorescent proteins as reporters.

  12. Gas chromatography of organic microcontaminants using atomic emission and mass spectrometric detection combined in one instrument (GC-AED/MS)

    NARCIS (Netherlands)

    Mol, H.G.J.; Hankemeier, T.; Brinkman, U.A.T.

    1999-01-01

    This study describes the coupling of an atomic-emission detector and mass-spectrometric detector to a single gas chromatograph. Splitting of the column effluent enables simultaneous detection by atomic-emission detection (AED) and mass spectrometry (MS) and yields a powerful system for the target an

  13. Containerless Atomic-Fluorescence Property Measurements

    Science.gov (United States)

    Nordine, P.; Schiffman, R.; Walker, C.

    1987-01-01

    Report describes studies conducted to establish and verify use of laser-induced fluorescence in monitoring and controlling high-temperature containerless processes. Specimens levitated by gas jets or electromagnetic fields and heated by laser beams or electromagnetic induction while being irradiated and detected by fluorescence technique. Makes quantitative and qualitative comparisons among three new methods of temperature measurement; all rely on laser-induced fluorescence. One method gas-density thermometry with seed gas. Other two methods involve measurements of velocities of evaporating atoms or of population ratios of different electronic states.

  14. 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.

  15. 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.

  16. Determination of cyanide by a flow injection analysis-atomic absorption spectrometric method.

    Science.gov (United States)

    López Gómez, A V; Martínez Calatayud, J

    1998-10-01

    A new flow injection analysis (FIA) procedure is proposed for the indirect atomic absorption spectrometric determination of cyanide. The FIA manifold is based on the insertion of the sample into a distilled water carrier, then the sample flows through a solid-phase reactor filled with silver iodide entrapped in polymeric resin beads. The calibration graph is linear over the range 0.2-6.0 mg l-1 of cyanide (correlation coefficient 0.9974), the detection limit is 0.1 mg l-1, the sample throughput is 193 h-1 and the RSD is 0.8%. The method is simple, quick and more selective than other published FIA procedures. The reproducibility obtained by using different solid-phase reactors and solutions is in the range 2.2-3.1% (RSD). The method was applied to the determination of cyanide in commercial samples such as pharmaceutical formulations and industrial electrolytic baths.

  17. 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.

  18. Atomic fluorescence study of high temperature aerodynamic levitation

    Science.gov (United States)

    Nordine, P. C.; Schiffman, R. A.; Sethi, D. S.

    1982-01-01

    Ultraviolet laser induced atomic fluorescence has been used to characterize supersonic jet aerodynamic levitation experiments. The levitated specimen was a 0.4 cm sapphire sphere that was separately heated at temperatures up to 2327 K by an infrared laser. The supersonic jet expansion and thermal gradients in the specimen wake were studied by measuring spatial variations in the concentration of atomic Hg added to the levitating argon gas stream. Further applications of atomic fluorescence in containerless experiments, such as ideal gas fluorescence thermometry and containerless process control are discussed.

  19. Containerless high temperature property measurements by atomic fluorescence

    Science.gov (United States)

    Nordine, P. C.; Schiffman, R. A.

    1982-01-01

    Laser induced fluorescence techniques were developed for the containerless study of high temperature processes, material properties, levitation, and heating techniques for containerless earth-based experimentation. Experiments were performed in which fluorescence of atomic aluminum, mercury, or tungsten were studied. These experiments include measurements of: (1) Al atom evaporation from CW CO2 laser heated and aerodynamically levitated sapphire and alumina spheres, and self-supported sapphire filaments, (2) Al atom reaction with ambient oxygen in the wake of a levitated specimen, (3) Hg atom concentrations in the wake of levitated alumina and sapphire spheres, relative to the ambient Hg atom concentration, (4) Hg atom concentrations in supersonic levitation jets, and (5) metastable, electronically excited W atom concentrations produced by evaporation of an electrically heated tungsten filament.

  20. Theory of analytical curves in atomic fluorescence flame spectrometry

    NARCIS (Netherlands)

    Hooymayers, H.P.

    1968-01-01

    An explicit expression for the intensity of atomic resonance fluorescence as a function of atomic concentration in a flame is derived under certain idealized conditions. The expression is generally valid for a pure Doppler absorption line profile as well as for a combined Doppler and collisional bro

  1. 基于差分吸收激光雷达的一种新的对流层臭氧浓度反演算法%Butanol Extraction Combined with Dilute Hydrochloric Acid Dissolution-Atomic Fluorescence Spectrometric Method for Indirect Determination of Molybdenum in Chinese Herbal Medicine

    Institute of Scientific and Technical Information of China (English)

    范广强; 刘建国; 刘文清; 陆亦怀; 张天舒; 董云升; 赵雪松

    2012-01-01

    A method for indirectly determining the molybdenum in Chinese herbal medicine by butanol extraction and dilute hydrochloric acid dissolution was established for atomic fluorescence spectrometry. The molybdoarsenate heteropoly acid, formed in the presence of As( V) and ammonium molybdate in 0. 3 mol · L-1 sulphuric acid medium, was separated and enriched in the organic solvent, then the evaporation of organic reagent was implemented and the left residue was dissolved in dilute hydrochloric acid in which the arsenic content was determined on behalf of molybdenum. In the optimum experimental conditions, molybdenum content in 0~15 μg · L-1 range depicts a good linear relationship, the detection limit and relative standard deviation of 0. 44 μg · L-1 and 1.1% were obtained, respectively. Spiked Chinese herbal medicine samples were determined with the proposed method, and recoveries of 95. 6%—101. 3% were achieved.%差分吸收激光雷达探测对流层臭氧浓度时,气溶胶的干扰会造成较大的误差.提出了一种算法,该算法能够同时反演得到对流层臭氧浓度和气溶胶消光系数,减少气溶胶对反演结果的影响.使用实验数据,分析计算了气溶胶雷达比,气溶胶波长指数、标定点气溶胶后向散射比各种变化参数对反演结果的误差.结果表明,1km以下,各种变化参数造成的反演误差小于8%,1km以上臭氧浓度误差主要来源于信号和背景噪声,各种参数反演误差小于3%.最后给出了利用该算法得到对流层臭氧浓度和气溶胶的消光系数垂直廓线,并和传统的双波长差分算法反演结果作了比较分析.实验结果表明该算法是可行的,该算法可以减少气溶胶对差分吸收激光雷达测量结果引起的误差.

  2. Study on Atomic Fluorescence Spectrometry Excited by Synchrotron Radiation

    Institute of Scientific and Technical Information of China (English)

    Jia-jia Guo; Wu-er Gan; Guo-bin Zhang; Qing-de Su

    2008-01-01

    A novel analysis approach using atomic fluorescence excited by synchrotron radiation is presented. A system for synchrotron radiation-atomic fluorescence spectrometry is developed, and experimental conditions such as flow rate, analyte acidity, concentration of pre-reducing and hydrogenation system are optimized. The proposed method is successfully applied to get an excitation spectrum of arsenic. Seven of ten primary spectral lines, four of which have never been reported by means of atomic fluorescence spectrometry, agree well with the existing reports. The other three are proposed for the first time. Excitation potentials and possible transitions are investigated. Especially for the prominent line at 234.99 nm, the mechanism of generation is discussed and a model of energy transition processes is proposed.

  3. Regime transition in electromechanical fluid atomization and implications to analyte ionization for mass spectrometric analysis.

    Science.gov (United States)

    Forbes, Thomas P; Degertekin, F Levent; Fedorov, Andrei G

    2010-11-01

    The physical processes governing the transition from purely mechanical ejection to electromechanical ejection to electrospraying are investigated through complementary scaling analysis and optical visualization. Experimental characterization and visualization are performed with the ultrasonically-driven array of micromachined ultrasonic electrospray (AMUSE) ion source to decouple the electrical and mechanical fields. A new dimensionless parameter, the Fenn number, is introduced to define a transition between the spray regimes, in terms of its dependence on the characteristic Strouhal number for the ejection process. A fundamental relationship between the Fenn and Strouhal numbers is theoretically derived and confirmed experimentally in spraying liquid electrolytes of different ionic strength subjected to a varying magnitude electric field. This relationship and the basic understanding of the charged droplet generation physics have direct implications on the optimal ionization efficiency and mass spectrometric response for different types of analytes.

  4. Driving the atom by atomic fluorescence: Analytic results for the power and noise spectra

    OpenAIRE

    2000-01-01

    We study how the spectral properties of resonance fluorescence propagate through a two-atom system. Within the weak-driving-field approximation we find that, as we go from one atom to the next, the power spectrum exhibits both subnatural linewidth narrowing and large asymmetries while the noise spectrum of the squeezed quadrature narrows but remains otherwise unchanged. Analytical results for the observed spectral features of the fluorescence are provided and their origin is thoroughly discus...

  5. 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.

  6. 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.

  7. Characterizing optical dipole trap via fluorescence of trapped cesium atoms

    Institute of Scientific and Technical Information of China (English)

    LIU Tao; GENG Tao; YAN Shubin; LI Gang; ZHANG Jing; WANG Junmin; PENG Kunchi; ZHANG Tiancai

    2006-01-01

    Optical dipole trap (ODT) is becoming an important tool of manipulating neutral atoms. In this paper ODT is realized with a far-off resonant laser beam strongly focused in the magneto-optical trap (MOT) of cesium atoms. The light shift is measured by simply monitoring the fluorescence of the atoms in the magneto-optical trap and the optical dipole trap simultaneously. The advantages of our experimental scheme are discussed, and the effect of the beam waist and power on the potential of dipole trap as well as heating rate is analyzed.

  8. Flame-in-gas-shield and miniature diffusion flame hydride atomizers for atomic fluorescence spectrometry: optimization and comparison

    OpenAIRE

    Marschner, K; Musil, S. (Stanislav); Dědina, J. (Jiří)

    2015-01-01

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH4 in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were ...

  9. Ultimate statistical physics: fluorescence of a single atom

    Science.gov (United States)

    Pomeau, Yves; Le Berre, Martine; Ginibre, Jean

    2016-10-01

    We discuss the statistics of emission of photons by a single atom or ion illuminated by a laser beam at the frequency of quasi-resonance between two energy levels, a situation that corresponds to real experiments. We extend this to the case of two laser beams resonant with the energy differences between two excited levels and the ground state (three level atom in V-configuration). We use a novel approach to this type of problem by considering a Kolmogorov equation for the probability distribution of the atomic state, which takes into account first the deterministic evolution of this state under the effect of the incoming laser beam and second the random emission of photons during the spontaneous decay of the excited state(s) to the ground state. This approach yields solvable equations in the two level atom case. For the three level atom case we set the problem and clearly define its frame. The results obtained are valid in both opposite limits of rare and frequent spontaneous decay, compared to the period of the optical Rabi oscillations due to the interaction between resonant excitation and atomic levels. Our analysis gives access to various statistical properties of the fluorescence light, including one showing that its fluctuations in time are not invariants under time reversal. This result makes evident the fundamentally irreversible character of quantum measurements, represented here by the emission of photons of fluorescence.

  10. Study on water-dispersible colloids in saline-alkali soils by atomic force microscopy and spectrometric methods.

    Science.gov (United States)

    Liu, Zhiguo; Xu, Fengjie; Zu, Yuangang; Meng, Ronghua; Wang, Wenjie

    2016-06-01

    Recent studies have revealed that water-dispersible colloids play an important role in the transport of nutrients and contaminants in soils. In this study, water-dispersible colloids extracted from saline-alkali soils have been characterized by atomic force microscopy (AFM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and UV absorption spectra. AFM observation indicated that the water-dispersible colloids contain some large plates and many small spherical particles. XRD, XPS, and UV absorption measurement revealed that the water-dispersible colloids are composed of kaolinite, illite, calcite, quartz and humic acid. In addition, UV absorption measurement demonstrated that the humic acids are associated with clay minerals. Water-dispersible colloids in the saline-alkali soils after hydrolyzed polymaleic anhydride treatment and an agricultural soil (nonsaline-alkali soil) were also investigated for comparison. The obtained results implied that the saline-alkali condition facilitates the formation of a large quantity of colloids. The use of AFM combined with spectrometric methods in the present study provides new knowledge on the colloid characteristics of saline-alkali soils. Microsc. Res. Tech. 79:525-531, 2016. © 2016 Wiley Periodicals, Inc.

  11. Elemental speciation analysis by multicapillary gas chromatography with microwave-induced plasma atomic spectrometric detection.

    Science.gov (United States)

    Rodriguez Pereiro, I; Schmitt, V O; Lobiński, R

    1997-12-01

    Multicapillary column gas chromatography (MC-GC)/microwave-induced plasma atomic emission spectrometry (MIP AES) was developed for fast speciation analysis of organotin compounds in the environment. Ethylated butyltin compounds could be separated isothermally within less than 30 s (instead of ∼5-10 min) without sacrificing either the resolution or the sample capacity of conventional capillary GC with oven temperature gradient programming. Careful optimization of the pressure and temperature GC program allowed a comprehensive organotin speciation analysis including phenyltin compounds within less than 2.5 min, increasing the sample throughput 6-fold. Compatibility of MC-GC with an MIP atomic emission detector (MIP-AED) was discussed. MC-GC/MIP-AES was validated for the analysis of sediment (PACS-1 and BCR 462) and biological (NIES11) certified reference materials.

  12. Resonance fluorescence of a trapped three-level atom

    CERN Document Server

    Bienert, M; Morigi, G; Bienert, Marc; Merkel, Wolfgang; Morigi, Giovanna

    2003-01-01

    We investigate theoretically the spectrum of resonance fluorescence of a harmonically trapped atom, whose internal transitions are $\\Lambda$--shaped and driven at two-photon resonance by a pair of lasers, which cool the center--of--mass motion. For this configuration, photons are scattered only due to the mechanical effects of the quantum interaction between light and atom. We study the spectrum of emission in the final stage of laser--cooling, when the atomic center-of-mass dynamics is quantum mechanical and the size of the wave packet is much smaller than the laser wavelength (Lamb--Dicke limit). We use the spectral decomposition of the Liouville operator of the master equation for the atomic density matrix and apply second order perturbation theory. We find that the spectrum of resonance fluorescence is composed by two narrow sidebands -- the Stokes and anti-Stokes components of the scattered light -- while all other signals are in general orders of magnitude smaller. For very low temperatures, however, th...

  13. 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.

  14. 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.

  15. SPE speciation of inorganic arsenic in rice followed by hydride-generation atomic fluorescence spectrometric quantification

    Science.gov (United States)

    Due to high toxicity, inorganic arsenics (iAs) are the focus of monitoring effort worldwide. In this work, extraction was performed by microwave-assisted digestion in HCl-H2O2, during which AsIII was oxidized to AsV. AsV was separated from organoarsenic species using silica-based SAX cartridge and r...

  16. Fluorescence Quenching of Benzaldehyde in Water by Hydrogen Atom Abstraction.

    Science.gov (United States)

    Fletcher, Katharyn; Bunz, Uwe H F; Dreuw, Andreas

    2016-09-01

    We computed the mechanism of fluorescence quenching of benzaldehyde in water through relaxed potential energy surface scans. Time-dependent density functional theory calculations along the protonation coordinate from water to benzaldehyde reveal that photoexcitation to the bright ππ* (S3 ) state is immediately followed by ultrafast decay to the nπ* (S1 ) state. Evolving along this state, benzaldehyde (BA) abstracts a hydrogen atom, resulting in a BAH(.) and OH(.) radical pair. Benzaldehyde does not act as photobase in water, but abstracts a hydrogen atom from a nearby solvent molecule. The system finally decays back to the ground state by non-radiative decay and an electron transfers back to the OH(.) radical. Proton transfer from BAH(+) to OH(-) restores the initial situation, BA in water.

  17. Single-atom-resolved fluorescence imaging of an atomic Mott insulator

    DEFF Research Database (Denmark)

    Sherson, Jacob; Weitenberg, Christof; Andres, Manuel;

    2010-01-01

    on the lattice and identify individual excitations with high fidelity. A comparison of the radial density and variance distributions with theory provides a precise in situ temperature and entropy measurement from single images. We observe Mott-insulating plateaus with near-zero entropy and clearly resolve...... in situ images of a quantum fluid in which each underlying quantum particle is detected. Here we report fluorescence imaging of strongly interacting bosonic Mott insulators in an optical lattice with single-atom and single-site resolution. From our images, we fully reconstruct the atom distribution...

  18. A sensitive fluorescence reagent for the determination of aldehydes from alcoholic beverage using high-performance liquid chromatography with fluorescence detection and mass spectrometric identification

    Energy Technology Data Exchange (ETDEWEB)

    You Jinmao [Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining 810001 (China)], E-mail: Jmyou6304@163.com; Yan Tao; Zhao Huaixin [Key Laboratory of Life-Organic Analysis, College of Chemistry Science, Qufu Normal University, Qufu Shandong 273165 (China); Sun Zhiwei; Xia Lian; Suo Yourui; Li Yulin [Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining 810001 (China)

    2009-03-16

    A pre-column derivatization method for the sensitive determination of aldehydes using the tagging reagent 2-[2-(7H-dibenzo[a,g] carbazol-7-yl)-ethoxy] ethyl carbonylhydrazine (DBCEEC) followed by high-performance liquid chromatography with fluorescence detection and APCI-MS identification has been developed. The chromophore of fluoren-9-methoxy-carbonylhydrazine (Fmoc-hydrazine) reagent was replaced by 2-[2-(7H-dibenzo[a,g] carbazol-7-yl)-ethoxy] ethyl functional group, which resulted in a sensitive fluorescence tagging reagent DBCEEC. DBCEEC could easily and quickly labeled aldehydes. The maximum excitation (300 nm) and emission (400 nm) wavelengths did not essentially change for all the aldehyde derivatives. Derivatives were sufficiently stable to be efficiently analyzed by high-performance liquid chromatography. The derivatives showed an intense protonated molecular ion corresponding m/z [M + (CH{sub 2}){sub n}]{sup +} in positive-ion mode (M: molecular weight of DBCEEC, n: corresponding aldehyde carbon atom numbers). The collision-induced dissociation of protonated molecular ion formed fragment ions at m/z 294.6, m/z 338.6 and m/z 356.5. Studies on derivatization demonstrated excellent derivative yields in the presence of trichloroacetic acid (TCA) catalyst. Maximal yields close to 100% were observed with a 10 to 15-fold molar reagent excess. Separation of the derivatized aldehydes had been optimized on ZORBAX Eclipse XDB-C{sub 8} column with aqueous acetonitrile as mobile phase in conjunction with a binary gradient elution. Excellent linear responses were observed at the concentration range of 0.01-10 nmol mL{sup -1} with coefficients of >0.9991. Detection limits obtained by the analysis of a derivatized standard containing 0.01 nmol mL{sup -1} of each aldehyde, were from 0.2 to 1.78 nmol L{sup -1} (at a signal-to-noise ratio of 3)

  19. Flame-in-gas-shield and miniature diffusion flame hydride atomizers for atomic fluorescence spectrometry: optimization and comparison

    Energy Technology Data Exchange (ETDEWEB)

    Marschner, Karel, E-mail: karel.marschner@biomed.cas.cz [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, Albertov 8, 128 43 Prague (Czech Republic); Musil, Stanislav; Dědina, Jiří [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

    2015-07-01

    A detailed optimization of relevant experimental parameters of two hydride atomizers for atomic fluorescence spectrometry: flame-in-gas-shield atomizer with a two-channel shielding unit and a standard atomizer for atomic fluorescence spectrometry, miniature diffusion flame, was performed. Arsine, generated by the reaction with NaBH{sub 4} in a flow injection arrangement, was chosen as the model hydride. Analytical characteristics of both the atomizers (sensitivity, noise, limits of detection) were compared. Under optimum conditions sensitivity obtained with flame-in-gas-shield atomizer was approximately twice higher than with miniature diffusion flame. The additional advantage of flame-in-gas-shield atomizer is significantly lower flame emission resulting in a better signal to noise ratio. The resulting arsenic limits of detection for miniature diffusion flame and flame-in-gas-shield atomizer were 3.8 ng l{sup −1} and 1.0 ng l{sup −1}, respectively. - Highlights: • We optimized and compared two hydride atomizers for atomic fluorescence spectrometry. • Miniature diffusion flame and flame-in-gas-shield atomizer were optimized. • The limit of detection for arsenic was 1.0 ng l{sup −1}.

  20. Flow injection on-line solid phase extraction for ultra-trace lead screening with hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Wan, Zhuo; Xu, Zhangrun; Wang, Jianhua

    2006-01-01

    A flow injection (FI) on-line solid phase extraction (SPE) procedure for ultra-trace lead separation and preconcentration was developed, followed by hydride generation and atomic fluorescence spectrometric (AFS) detection. Lead is retained on an iminodiacetate chelating resin packed microcolumn, and is afterward eluted with 2.5% (v/v) hydrochloric acid to facilitate the hydride generation by reaction with alkaline tetrahydroborate solution with 1% (m/v) potassium ferricyanide as an oxidizing (or sensitizing) reagent. The hydride was separated from the reaction medium in the gas-liquid separator and swept into the atomizer for quantification. The chemical variables and the FI flow parameters were carefully optimized. With a sample loading volume of 4.8 ml, quantitative retention of lead was obtained, along with an enrichment factor of 11.3 and a sampling frequency of 50 h(-1). A detection limit of 4 ng l(-1), defined as 3 times the blank standard deviation (3 sigma), was achieved along with a RSD value of 1.6% at the 0.4 microg l(-1) level. The procedure was validated by determining lead contents in two certified reference materials, and its practical applicability was further demonstrated by analysing a variety of biological and environmental samples.

  1. Influence of angle's ranges for recording an X-ray fluorescence hologram on reconstructed atomic images

    Institute of Scientific and Technical Information of China (English)

    XIE Hong-Lan; CHEN Jian-Wen; GAO Hong-Yi; ZHU Hua-Feng; LI Ru-Xin; XU Zhi-Zhan

    2004-01-01

    X-ray fluorescence holography (XFH) is a novel method for three-dimensional (3D) imaging of atomic structure. Theoretically, in an XFH experiment, one has to measure the fluorescence energy on a spherical surface to get well-resolved 3D images of atoms. But in practice, the experimental system arrangement does not allow the measurement of the fluorescent intensity oscillations in the full sphere. The holographic information losses because of the limited sampling range (less than 4π) will directly result in defective reconstructed atomic images. In this work, the atomic image of a Fe single crystal (001) was reconstructed by numerically simulating X-ray fluorescence holograms of the crystal at different recording angle's ranges and step lengths. Influences of the ranges of azimuth angles and polar angles and the step length of polar angles on the reconstructed atomic images were discussed.

  2. Development of off-line layer chromatographic and total reflection X-ray fluorescence spectrometric methods for arsenic speciation

    Energy Technology Data Exchange (ETDEWEB)

    Mihucz, Victor G. [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); Moricz, Agnes M. [L. Eoetvoes University, Department of Chemical Technology and Environmental Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Kroepfl, Krisztina [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Szikora, Szilvia [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary); Tatar, Eniko [Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary); L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary); Parra, Lue Meru Marco [Universidad Centro-occidental Lisandro Alvarado, Decanato de Agronomia, Departamento de Quimica y Suelos Unidad de Analisis Instrumental, Apartado Postal 4076, Cabudare 3023 (Venezuela); Zaray, Gyula [Joint Research Group of Environmental Chemistry of Hungarian Academy of Sciences and L. Eoetvoes University, P. O. Box 32, H-1518 Budapest (Hungary) and Hungarian Satellite Centre of Trace Elements Institute to UNESCO, P. O. Box 32, H-1518 Budapest (Hungary) and L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, H-1518 Budapest (Hungary)]. E-mail: zaray@ludens.elte.hu

    2006-11-15

    Rapid and low cost off-line thin layer chromatography-total reflection X-ray fluorescence spectrometry and overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods have been developed for separation of 25 ng of each As(III), As(V), monomethyl arsonic acid and dimethylarsinic acid applying a PEI cellulose stationary phase on plastic sheets and a mixture of acetone/acetic acid/water = 2:1:1 (v/v/v) as eluent system. The type of eluent systems, the amounts (25-1000 ng) of As species applied to PEI cellulose plates, injection volume, development distance, and flow rate (in case of overpressured thin layer chromatography) were taken into consideration for the development of the chromatographic separation. Moreover, a microdigestion method employing nitric acid for the As spots containing PEI cellulose scratched from the developed plates divided into segments was developed for the subsequent total reflection X-ray fluorescence spectrometry analysis. The method was applied for analysis of root extracts of cucumber plants grown in As(III) containing modified Hoagland nutrient solution. Both As(III) and As(V) were detected by applying the proposed thin layer chromatography/overpressured thin layer chromatography-total reflection X-ray fluorescence spectrometry methods.

  3. Two-photon-excited fluorescence spectroscopy of atomic fluorine at 170 nm

    Science.gov (United States)

    Herring, G. C.; Dyer, Mark J.; Jusinski, Leonard E.; Bischel, William K.

    1988-01-01

    Two-photon-excited fluorescence spectroscopy of atomic fluorine is reported. A doubled dye laser at 286-nm is Raman shifted in H2 to 170 nm (sixth anti-Stokes order) to excite ground-state 2P(0)J fluorine atoms to the 2D(0)J level. The fluorine atoms are detected by one of two methods: observing the fluorescence decay to the 2PJ level or observing F(+) production through the absorption of an additional photon by the excited atoms. Relative two-photon absorption cross sections to and the radiative lifetimes of the 2D(0)J states are measured.

  4. Double-well atom trap for fluorescence detection at the Heisenberg limit

    Science.gov (United States)

    Stroescu, Ion; Hume, David B.; Oberthaler, Markus K.

    2015-01-01

    We experimentally demonstrate an atom number detector capable of simultaneous detection of two mesoscopic ensembles with single-atom resolution. Such a sensitivity is a prerequisite for quantum metrology at a precision approaching the Heisenberg limit. Our system is based on fluorescence detection of atoms in a hybrid trap in which a dipole barrier divides a magneto-optical trap into two separated wells. We introduce a noise model describing the various sources contributing to the measurement error and report a limit of up to 500 atoms for single-atom resolution in the atom number difference.

  5. Saturation of Energy Levels in Analytical Atomic Fluorescence Spectrometry. II. Experimental.

    Science.gov (United States)

    1981-01-30

    RESEARCH Contract N14-76-C-0838 Task Ao. NR 051-622 TECHNICAL REPORT NO. 34 SATURATION OF ENERGY LEVELS IN ANALYTICAL ATOMIC FLUORESCENCE SPECTROMETRY II...an assumption which is valid only if the daral o’l of 111, cxcilIatio n pulse is mucl ) longer than the fluorescence life- time of the tjaii!,ition

  6. A double-well atom trap for fluorescence detection at the Heisenberg limit

    CERN Document Server

    Stroescu, Ion; Oberthaler, Markus K

    2014-01-01

    We experimentally demonstrate an atom number detector capable of simultaneous detection of two mesoscopic ensembles with single atom resolution. Such a sensitivity is a prerequisite for going beyond quantum metrology with spin-squeezed states. Our system is based on fluorescence detection of atoms in a novel hybrid trap in which a dipole barrier divides a magneto-optical trap into two separated wells. We introduce a noise model describing the various sources contributing to the measurement error and report a limit of up to 500 atoms for the exact determination of the atom number difference.

  7. Resonance fluorescence of a cold atom in a high-finesse resonator

    CERN Document Server

    Bienert, M; Torres, J M; Zippilli, S; Bienert, Marc; Morigi, Giovanna; Zippilli, Stefano

    2007-01-01

    We study the spectra of emission of a system composed by an atom, tightly confined inside a high-finesse resonator, when the atom is driven by a laser and is at steady state of the cooling dynamics induced by laser and cavity field. In general, the spectrum of resonance fluorescence and the spectrum at the cavity output contain complementary information about the dynamics undergone by the system. In certain parameter regimes, quantum interference effects between the scattering processes induced by cavity and laser field lead to the selective suppression of features of the resonance fluorescence spectrum, which are otherwise visible in the spectrum of laser-cooled atoms in free space.

  8. Simple and sensitive determination of o-phenylphenol in citrus fruits using gas chromatography with atomic emission or mass spectrometric detection.

    Science.gov (United States)

    Kolbe, Nina; Andersson, Jan T

    2006-08-09

    In this work, a simple and sensitive method for the analysis of the pesticide o-phenylphenol (OPP) on citrus fruits was developed. OPP is extracted with dichloromethane by ultrasonication and derivatized with ferrocenecarboxylic acid chloride. Using ferrocene as a label, residues of OPP are determined by gas chromatography with atomic emission detection in the iron selective mode or with mass spectrometric detection. Sample cleanup is simple and rapid and merely involves a removal of excess reagent on an alumina minicolumn. The method detection limit is 2 ng of OPP/g of fruit, and recoveries from lemon samples fortified at levels of 35 and 140 ng/g are 101 and 106%, respectively. The citrus fruits analyzed (oranges, grapefruits, lemons) contained between 60 ng/g and 0.37 microg/g OPP (RSD = 8-13%), and the results were in good agreement with results obtained when OPP was analyzed using an established HPLC-FLD method. Several alcohols could also be identified in the fruit peel.

  9. Cooperative fluorescence from a strongly driven dilute cloud of atoms

    DEFF Research Database (Denmark)

    Ott, Johan Raunkjær; Wubs, Martijn; Lodahl, Peter;

    2013-01-01

    We investigate cooperative fluorescence in a dilute cloud of strongly driven two-level emitters. Starting from the Heisenberg equations of motion, we compute the first-order scattering corrections to the saturation of the excited-state population and to the resonance-fluorescence spectrum, which...... both require going beyond the state-of-the-art linear-optics approach to describe collective phenomena. A dipole blockade is observed due to long-range dipole-dipole coupling that vanishes at stronger driving fields. Furthermore, we compute the inelastic component of the light scattered by a cloud...

  10. Ultimate Statistical Physics: fluorescence of a single atom

    CERN Document Server

    Pomeau, Yves; Ginibre, Jean

    2016-01-01

    We discuss the statistics of emission of photons by a single atom or ion illuminated by a laser beam at the frequency of quasi-resonance between two energy levels, a situation that corresponds to real experiments. We extend this to the case of two laser beams resonant with the energy differences between two excited levels and the ground state (three level atom in V-configuration). We use a novel approach of this type of problem by considering Kolmogorov equation for the probability distribution of the atomic state which takes into account first the deterministic evolution of this state under the effect of the incoming laser beam and the random emission of photons during the spontaneous decay of the excited state(s) to the ground state. This approach yields solvable equations in the two level atom case. For the three level atom case we set the problem and define clearly its frame. The results obtained are valid both in the opposite limits of rare and of frequent spontaneous decay, compared to the period of the...

  11. In-trap fluorescence detection of atoms in a microscopic dipole trap

    CERN Document Server

    Hilliard, A J; Sompet, P; Carpentier, A V; Andersen, M F

    2015-01-01

    We investigate fluorescence detection using a standing wave of blue-detuned light of one or more atoms held in a deep, microscopic dipole trap. The blue-detuned standing wave realizes a Sisyphus laser cooling mechanism so that an atom can scatter many photons while remaining trapped. When imaging more than one atom, the blue detuning limits loss due to inelastic light-assisted collisions. Using this standing wave probe beam, we demonstrate that we can count from one to the order of 100 atoms in the microtrap with sub-poissonian precision.

  12. Atomic force fluorescence microscopy : combining the best of two worlds

    NARCIS (Netherlands)

    Kassies, Roelf

    2005-01-01

    The complementary strengths and weaknesses of AFM and optical microscopy leads to the desire to integrate both techniques into a single microscope. This thesis describes the development of a com-bined AFM / confocal °uorescence microscope. This atomic force °uorescence microscope (AFFM) combines hig

  13. 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.

  14. 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.

  15. Membrane filtration of nickel(II) on cellulose acetate filters for its preconcentration, separation, and flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Soylak, Mustafa [Chemistry Dept., Faculty of Science Arts, University of Erciyes, Kayseri (Turkey); Unsal, Yunus Emre; Aydin, Ayse [Fen Bilimleri Enstitusu, University of Erciyes, Kayseri (Turkey); Kizil, Nebiye [Saglik Bilimleri Enstitusu, University of Erciyes, Kayseri (Turkey)

    2010-01-15

    An enrichment method for trace amounts of Ni(II), as 8-hydroxyquinoline chelates, has been established on a cellulose acetate membrane filter. Ni(II)-8-hydroxyquinoline chelates adsorbed on a membrane filter were eluted using 5 mL of 1 M HNO{sub 3}. The eluent nickel concentration was determined by a flame atomic absorption spectrometer. The influence of some analytical parameters, including pH, amount of reagent, sample volume, etc., on recovery was investigated. The interference of co-existent ions was studied. The nickel detection limit was 4.87 {mu}g/L. The method was applied to real samples for the determination of nickel(II) ions. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  16. Solid phase extraction of gold(III) on Amberlite XAD-2000 prior to its flame atomic absorption spectrometric determination.

    Science.gov (United States)

    Elci, Latif; Sahan, Derya; Basaran, Aydan; Soylak, Mustafa

    2007-09-01

    A solid phase extraction method for the determination of gold(III) at trace levels by flame atomic absorption spectrometer (FAAS) was developed. The method was based on retention of gold as chloro complexes through the Amberlite XAD-2000. The effect of some analytical parameters including hydrochloric acid concentration, sample volume, sample and eluent flow rates, eluent volume, eluent concentration and interfering ions on the recovery of gold(III) was investigated. The retention of gold(III) from 1.5 mol l(-1) HCl solution and the recovery of gold with 0.07 mol l(-1) NH3 solution were quantitative (>or=95%). The relative standard deviation (RSD) was calculated as 3.2% (n = 10). The detection limit for gold was 2 microg l(-1). The accuracy was checked with the determination of gold spiked an artificial seawater and a pure copper samples.

  17. 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...

  18. On-line preconcentration of copper as its pyrocatechol violet complex on Chromosorb 105 for flame atomic absorption spectrometric determinations

    Energy Technology Data Exchange (ETDEWEB)

    Buke, Berrin [Chemistry Department, Science and Arts Faculty, Pamukkale University, 20020 Denizli (Turkey); Divrikli, Umit [Chemistry Department, Science and Arts Faculty, Pamukkale University, 20020 Denizli (Turkey)], E-mail: udivrikli@pamukkale.edu.tr; Soylak, Mustafa [Chemistry Department, Science and Arts Faculty, Erciyes University, 38039 Kayseri (Turkey); Elci, Latif [Chemistry Department, Science and Arts Faculty, Pamukkale University, 20020 Denizli (Turkey)

    2009-04-30

    An on-line solid phase extraction method for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry (FAAS) has been described. It is based on the adsorption of copper(II) ion onto a home made mini column of Chromosorb 105 resin loaded with pyrocatechol violet at the pH range of 5.0-8.0, then eluted with 1 mol L{sup -1} HNO{sub 3}. Several parameters, such as pH of the sample solution, amount of Chromosorb 105 resin, volume of sample and eluent, type of eluent, flow rates of sample and eluent, governing the efficiency and throughput of the method were evaluated. The concentration of the copper ion detected after preconcentration was in agreement with the added amount. At optimized conditions, for 15 min of preconcentration time (30 mL of sample volume), the system achieved a detection limit of 0.02 {mu}g L{sup -1}, with relative standard deviation 1.1% at 0.03 {mu}g mL{sup -1} copper. The present method was found to be applicable to the preconcentration of Cu(II) in natural water samples.

  19. Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Senturk, Hasan Basri; Gundogdu, Ali [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 28049 Giresun (Turkey); Duran, Celal [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Arts and Sciences, Pamukkale University, 20020 Denizli (Turkey); Tufekci, Mehmet [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)

    2007-10-22

    A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L{sup -1} HNO{sub 3} in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 {mu}g L{sup -1}, respectively. The preconcentration factor was 200. The relative standard deviation of the method was <6%. The adsorption capacity of the resin was 12.3 mg g{sup -1}. The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples.

  20. 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.

  1. Separation of gold, palladium and platinum in chromite by anion exchange chromatography for inductively coupled plasma atomic emission spectrometric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Kwang Soon; Lee, Chang Heon; Park, Yeong Jae; Joe, Kih Soo; Kim, Won Ho [KAERI, Taejon (Korea, Republic of)

    2001-08-01

    A study has been carried out on the separation of gold, iridium, palladium, rhodium, ruthenium and platinum in chromite samples and their quantitative determination using inductively coupled plasma atomic emission spectrometry (ICP-AES). The dissolution condition of the minerals by fusion with sodium peroxide was optimized and chromatographic elution behavior of the rare metals was investigated by anion exchange chromatography. Spectral interference of chromium, a matrix of the minerals, was investigated on determination of gold. Chromium interfered on determination of gold at the concentration of 500 mg/L and higher. Gold plus trace amounts of iridium, palladium, rhodium and ruthenium, which must be preconcentrated before ICP-AES was separated by anion exchange chromatography after reducing Cr(VI) to Cr(III) by H{sub 2}O{sub 2}. AuCl{sup -}{sub 4} retained on the resin column was selectively eluted with acetone- HNO{sub 3}-H{sub 2}O as an eluent. In addition, iridium, palladium, rhodium and ruthenium remaining on the resin column were eluted as a group with concentrated HCl. However, platinum was eluted with concentrated HNO{sub 3}. The recovery yield of gold with acetone-HNO{sub 3}-H{sub 2}O was 100.7 {+-} 2.0 % , and the yields of palladium and platinum with concentrated HCl and HNO{sub 3} were 96.1 {+-} 1.8% and 96.6 {+-} 1.3%, respectively. The contents of gold and platinum in a Mongolian chromite sample were 32.6 {+-} 2.2 {mu}g/g and 1.6 {+-} 0.14 {mu}g/g, respectively. Palladium was not detected.

  2. 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.

  3. Observation of DNA Molecules Using Fluorescence Microscopy and Atomic Force Microscopy

    Science.gov (United States)

    Ito, Takashi

    2008-01-01

    This article describes experiments for an undergraduate instrumental analysis laboratory that aim to observe individual double-stranded DNA (dsDNA) molecules using fluorescence microscopy and atomic force microscopy (AFM). dsDNA molecules are observed under several different conditions to discuss their chemical and physical properties. In…

  4. Polymerized LB films imaged with a combined atomic force microscope-fluorescence microscope

    NARCIS (Netherlands)

    Putman, Constant A.J.; Hansma, Helen G.; Gaub, Hermann E.; Hansma, Paul K.

    1992-01-01

    The first results obtained with a new stand-alone atomic force microscope (AFM) integrated with a standard Zeiss optical fluorescence microscope are presented. The optical microscope allows location and selection of objects to be imaged with the high-resolution AFM. Furthermore, the combined microsc

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

    Energy Technology Data Exchange (ETDEWEB)

    Miró, Manuel, E-mail: manuel.miro@uib.es [FI-TRACE Group, Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, E-07122 Palma de Mallorca, Illes Balears (Spain); Hansen, Elo Harald [Granåsen 93, DK-2800 Kgs. Lyngby (Denmark)

    2013-06-11

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

  6. Far-field resonance fluorescence from a dipole-interacting laser-driven cold atomic gas

    Science.gov (United States)

    Jones, Ryan; Saint, Reece; Olmos, Beatriz

    2017-01-01

    We analyze the temporal response of the fluorescence light that is emitted from a dense gas of cold atoms driven by a laser. When the average interatomic distance is comparable to the wavelength of the photons scattered by the atoms, the system exhibits strong dipolar interactions and collective dissipation. We solve the exact dynamics of small systems with different geometries and show how these collective features are manifest in the scattered light properties such as the photon emission rate, the power spectrum and the second-order correlation function. By calculating these quantities beyond the weak (linear) driving limit, we make progress in understanding the signatures of collective behavior in these many-body systems. Furthermore, we shed light on the role of disorder and averaging on the resonance fluorescence, of direct relevance for recent experimental efforts that aim at the exploration of many-body effects in dipole-dipole interacting gases of atoms.

  7. Comparative mass spectrometric analyses of Photofrin oligomers by fast atom bombardment mass spectrometry, UV and IR matrix-assisted laser desorption/ionization mass spectrometry, electrospray ionization mass spectrometry and laser desorption/jet-cooling photoionization mass spectrometry.

    Science.gov (United States)

    Siegel, M M; Tabei, K; Tsao, R; Pastel, M J; Pandey, R K; Berkenkamp, S; Hillenkamp, F; de Vries, M S

    1999-06-01

    Photofrin (porfimer sodium) is a porphyrin derivative used in the treatment of a variety of cancers by photodynamic therapy. This oligomer complex and a variety of porphyrin monomers, dimers and trimers were analyzed with five different mass spectral ionization techniques: fast atom bombardment, UV and IR matrix-assisted laser desorption/ionization, electrospray ionization, and laser desorption/jet-cooling photoionization. All five approaches resulted in very similar oligomer distributions with an average oligomer length of 2.7 +/- 0.1 porphyrin units. In addition to the Photofrin analysis, this study provides a side-by-side comparison of the spectra for the five different mass spectrometric techniques.

  8. [Investigation of enhancing effect for hydride generation-atomic fluorescence of transition metal elements].

    Science.gov (United States)

    Sun, Han-Wen; Suo, Ran

    2008-11-01

    A mechanism of hydride generation based on disassembly reaction of hydrogen-transferred interim state [M(BH4)m]* was developed by investigating the effect of reaction medium acidity on hydride generation. The effects of Co2+ and Ni2+, phenanthroline and 8-hydroxyquinoline on hydride generation-atomic fluorescence signals of Zn, Cd, Cu and Ni were studied, respectively, and their enhancing mechnism was discussed. The enhancing effect Co2+ and Ni2+ on the fluorescence signals of Zn and Cd was due to the increase in transmission efficiency of hydride of Zn and Cd. There was a synergic enhancing effect between phenanthroline or 8-hydroxyquinoline and Co2+ on the fluorescence signals of Zn and Cd, however no synergic enhancing effect between phenanthroline and 8-hydroxyquinoline on the fluorescence signals of Zn and Cd. The simulative action of cationic surfactant, anion surfactant and non-ionic surfactant surfactant to hydride generation was investigated. It is shown that both cationic surfactant and non-ionic surfactant have obvious enhancing effect on the fluorescence signals of analytes because of the decrease in surface tension of reaction solution. The release characteristics of hydride from the absorption solution containing surfactant was ulteriorly examined by using graphite furnace atomic absorption spectrometry, and the mechanism of enhancing effect of surfactant on hydride generation and transmission was proposed.

  9. The determination of major and some minor constituents in lead zirconate-titanate compositions by x-ray fluorescence and atomic absorption spectrometry

    NARCIS (Netherlands)

    Willigen, van J.H.H.G.; Kruidhof, H.; Dahmen, E.A.M.F.

    1972-01-01

    An accurate X-ray fluorescence spectrometric method is described for the determination of lead, zirconium and titanium in lead zirconate-titanate ceramics. Careful matching of samples and standards by a borax fusion method resulted in a relative standard deviation of about 0.2% for the major constit

  10. Phase Dependence of Fluorescence Spectrum of a Two-Level Atom in a Trichromatic Field

    Institute of Scientific and Technical Information of China (English)

    LI Jing-Yan; HU Xiang-Ming; LI Xiao-Xia; SHI Wen-Xing; XU Qing; GUO Hong-Ju

    2005-01-01

    @@ We examine the phase-dependent effects in resonance fluorescence of a two-level atom driven by a trichromatic modulated field. It is shown that the fluorescence spectrum depends crucially on the sum of relative phases of the sideband components compared to the central component, not simply on the respective phases. The appearance or disappearance of the central peak and the selective elimination of the sideband peaks are achieved simply by varying the sum phase. Once the sum phase is fixed, the spectrum keeps its features unchanged regardless of the respective relative phases.

  11. Colorful Polyelectrolytes: An Atom Transfer Radical Polymerization Route to Fluorescent Polystyrene Sulfonate.

    Science.gov (United States)

    Huberty, Wayne; Tong, Xiaowei; Balamurugan, Sreelatha; Deville, Kyle; Russo, Paul S; Zhang, Donghui

    2016-03-01

    A labeled green fluorescent polystyrene sulfonate (LNaPSS) has been synthesized using atom transfer radical polymerization of a styrene sulfonate monomer with a fluorescent co-monomer, fluorescein thiocyanate-vinyl aniline. As a result this 100 % sulfonated polymer contains no hydrophobic patches along the chain backbone besides the fluorescent marker itself. The concentration of the fluorescent monomer was kept low to maintain the characteristic properties of the anionic polyelectrolyte, LNaPSS. ATRP conditions facilitated the production of polymers spanning a range of molecular weights from 35,000 to 175,000 in gram-scale batches with polydispersity indices of 1.01-1.24. Molecular weight increased with the monomer to initiator ratio. Gel permeation chromatography results show a unimodal distribution, and the polymer structure was also confirmed by (1)H NMR and FT-IR spectroscopy. Fluorescence spectroscopy confirmed covalent bonding of fluorescein isothiocyanate to the polymer, indicating that the polymer is suitable as a probe in fluorescence microscopy. To demonstrate this ability, the polymer was used to locate structural features in salt crystals formed during drying, as in the evaporation of sea mist. A second application to probe diffusion studies is also demonstrated.

  12. Fluorescence (TALIF) measurement of atomic hydrogen concentration in a coplanar surface dielectric barrier discharge

    Science.gov (United States)

    Mrkvičková, M.; Ráheľ, J.; Dvořák, P.; Trunec, D.; Morávek, T.

    2016-10-01

    Spatially and temporally resolved measurements of atomic hydrogen concentration above the dielectric of coplanar barrier discharge are presented for atmospheric pressure in 2.2% H2/Ar. The measurements were carried out in the afterglow phase by means of two-photon absorption laser-induced fluorescence (TALIF). The difficulties of employing the TALIF technique in close proximity to the dielectric surface wall were successfully addressed by taking measurements on a suitable convexly curved dielectric barrier, and by proper mathematical treatment of parasitic signals from laser-surface interactions. It was found that the maximum atomic hydrogen concentration is situated closest to the dielectric wall from which it gradually decays. The maximum absolute concentration was more than 1022 m-3. In the afterglow phase, the concentration of atomic hydrogen above the dielectric surface stays constant for a considerable time (10 μs-1 ms), with longer times for areas situated farther from the dielectric surface. The existence of such a temporal plateau was explained by the presented 1D model: the recombination losses of atomic hydrogen farther from the dielectric surface are compensated by the diffusion of atomic hydrogen from regions close to the dielectric surface. The fact that a temporal plateau exists even closest to the dielectric surface suggests that the dielectric surface acts as a source of atomic hydrogen in the afterglow phase.

  13. Communication: angular momentum alignment and fluorescence polarization of alkali atoms photodetached from helium nanodroplets.

    Science.gov (United States)

    Hernando, Alberto; Beswick, J Alberto; Halberstadt, Nadine

    2013-12-14

    The theory of photofragments angular momentum polarization is applied to the photodetachment of an electronically excited alkali atom from a helium nanocluster (N = 200). The alignment of the electronic angular momentum of the bare excited alkali atoms produced is calculated quantum mechanically by solving the excited states coupled equations with potentials determined by density functional theory (DFT). Pronounced oscillations as a function of excitation energy are predicted for the case of Na@(He)200, in marked contrast with the absorption cross-section and angular distribution of the ejected atoms which are smooth functions of the energy. These oscillations are due to quantum interference between different coherently excited photodetachment pathways. Experimentally, these oscillations should be reflected in the fluorescence polarization and polarization-resolved photoelectron yield of the ejected atoms, which are proportional to the electronic angular momentum alignment. In addition, this result is much more general than the test case of NaHe200 studied here. It should be observable for larger droplets, for higher excited electronic states, and for other alkali as well as for alkali-earth atoms. Detection of these oscillations would show that the widely used pseudo-diatomic model can be valid beyond the prediction of absorption spectra and could help in interpreting parts of the dynamics, as already hinted by some experimental results on angular anisotropy of bare alkali fragments.

  14. Communication: Angular momentum alignment and fluorescence polarization of alkali atoms photodetached from helium nanodroplets

    Energy Technology Data Exchange (ETDEWEB)

    Hernando, Alberto; Beswick, J. Alberto; Halberstadt, Nadine [LCAR-IRSAMC, Université Toulouse 3 - Paul Sabatier and CNRS, 31062 Toulouse (France)

    2013-12-14

    The theory of photofragments angular momentum polarization is applied to the photodetachment of an electronically excited alkali atom from a helium nanocluster (N = 200). The alignment of the electronic angular momentum of the bare excited alkali atoms produced is calculated quantum mechanically by solving the excited states coupled equations with potentials determined by density functional theory (DFT). Pronounced oscillations as a function of excitation energy are predicted for the case of Na@(He){sub 200}, in marked contrast with the absorption cross-section and angular distribution of the ejected atoms which are smooth functions of the energy. These oscillations are due to quantum interference between different coherently excited photodetachment pathways. Experimentally, these oscillations should be reflected in the fluorescence polarization and polarization-resolved photoelectron yield of the ejected atoms, which are proportional to the electronic angular momentum alignment. In addition, this result is much more general than the test case of NaHe{sub 200} studied here. It should be observable for larger droplets, for higher excited electronic states, and for other alkali as well as for alkali-earth atoms. Detection of these oscillations would show that the widely used pseudo-diatomic model can be valid beyond the prediction of absorption spectra and could help in interpreting parts of the dynamics, as already hinted by some experimental results on angular anisotropy of bare alkali fragments.

  15. Arsenic species analysis in porewaters and sediments using hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    LIAO Meng-xia; DENG Tian-long

    2006-01-01

    It was observed that the atomic fluorescence emission due to As(Ⅴ) could has a 10% to 40% of fluorescence emission signal during the determination of As(Ⅲ) in the mixture of As(Ⅲ) and As(Ⅴ). Besides, interferes from heavy metals such as Pb(Ⅱ),Cu(Ⅱ) can cause severe increase of the signals as compared to the insignificant effects caused by Cd(Ⅱ), Zn(Ⅱ), Mn(Ⅱ) and Fe(Ⅲ). On the basis of further studies, the masking agent of 8-hydroxyquinoline was used as an efficient agent to eliminate interference of As(Ⅴ)emission and the heavy metal of Cu2+ and Pb2+ in the measurements of arsenic species. After a series standard additions and CRM researches, a sensitive and interference-free analytical procedure was developed for the speciation of arsenic in samples ofporewaters and sediments in Poyang Lake, China.

  16. Sub-cellular structure studied by combined atomic force-fluorescence microscopy

    Science.gov (United States)

    Trache, Andreea

    2009-03-01

    A novel experimental technique that integrates atomic force microscopy (AFM) with fluorescence imaging was used to study the role of extracellular matrix proteins in cellular organization. To understand the mechanism by which living cells sense mechanical forces, and how they respond and adapt to their environment, we developed a new technology able to investigate cellular behavior at sub-cellular level that integrates an AFM with total internal reflection fluorescence (TIRF) microscopy and fast-spinning disk (FSD) confocal microscopy. Live smooth muscle cells exhibited differences in focal adhesions and actin pattern depending on the extracellular matrix used for substrate coating. Data obtained by using the AFM-optical imaging integrated technique offer novel quantitative information that allows understanding the fundamental processes of cellular reorganization in response to extracellular matrix modulation. The integrated microscope presented here is broadly applicable across a wide range of molecular dynamic studies in any adherent live cells.

  17. 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.

  18. 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%.

  19. Real-time near-field terahertz imaging with atomic optical fluorescence

    Science.gov (United States)

    Wade, C. G.; Šibalić, N.; de Melo, N. R.; Kondo, J. M.; Adams, C. S.; Weatherill, K. J.

    2017-01-01

    Terahertz (THz) near-field imaging is a flourishing discipline, with applications from fundamental studies of beam propagation to the characterization of metamaterials and waveguides. Beating the diffraction limit typically involves rastering structures or detectors with length scale shorter than the radiation wavelength; in the THz domain this has been achieved using a number of techniques including scattering tips and apertures. Alternatively, mapping THz fields onto an optical wavelength and imaging the visible light removes the requirement for scanning a local probe, speeding up image collection times. Here, we report THz-to-optical conversion using a gas of highly excited Rydberg atoms. By collecting THz-induced optical fluorescence we demonstrate a real-time image of a THz standing wave and use well-known atomic properties to calibrate the THz field strength.

  20. Electrochemical hydride generation atomic fluorescence spectrometry for detection of tin in canned foods using polyaniline-modified lead cathode.

    Science.gov (United States)

    Jiang, Xianjuan; Gan, Wuer; Wan, Lingzhong; Deng, Yun; Yang, Qinghua; He, Youzhao

    2010-12-15

    An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH(4) and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL(-1) (3σ) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL(-1) Sn(IV) standard solution.

  1. Development of a 2D temperature measurement technique for combustion diagnostics using 2-line atomic fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Engstroem, Johan

    2001-01-01

    The present thesis is concerned with the development and application of a novel planar laser-induced fluorescence (PLIF) technique for temperature measurements in a variety of combusting flows. Accurate measurement of temperature is an essential task in combustion diagnostics, since temperature is one of the most fundamental quantities for the characterization of combustion processes. The technique is based on two-line atomic fluorescence (TLAF) from small quantities of atomic indium (In) seeded into the fuel. It has been developed from small-scale experiments in laboratory flames to the point where practical combustion systems can be studied. The technique is conceptually simple and reveals temperature information in the post-flame regions. The viability of the technique has been tested in three extreme measurement situations: in spark ignition engine combustion, in ultra-lean combustion situations such as lean burning aero-engine concepts and, finally, in fuel-rich combustion. TLAF was successfully applied in an optical Sl engine using isooctane as fuel. The wide temperature sensitivity, 700 - 3000 K, of the technique using indium atoms allowed measurements over the entire combustion cycle in the engine to be performed. In applications in lean combustion a potential problem caused by the strong oxidation processes of indium atoms was encountered. This limits measurement times due to deposits of absorbing indium oxide on measurement windows. The seeding requirement is a disadvantage of the technique and can be a limitation in some applications. The results from experiments performed in sooting flames are very promising for thermometry measurements in such environments. Absorption by hydrocarbons and other native species was found to be negligible. Since low laser energies and low seeding concentrations could be used, the technique did not, unlike most other incoherent optical thermometry techniques, suffer interferences from LII of soot particles or LIF from PAH

  2. 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

  3. Pressure broadening of atomic oxygen two-photon absorption laser induced fluorescence

    Science.gov (United States)

    Marinov, Daniil; Drag, Cyril; Blondel, Christophe; Guaitella, Olivier; Golda, Judith; Klarenaar, Bart; Engeln, Richard; Schulz-von der Gathen, Volker; Booth, Jean-Paul

    2016-12-01

    Atomic oxygen, considered to be a determining reactant in plasma applications at ambient pressure, is routinely detected by two-photon absorption laser induced fluorescence (TALIF). Here, pressure broadening of the (2p 4 3 P 2  →  3p 3 P J=0,1,2) two-photon transition in oxygen atoms was investigated using a high-resolution TALIF technique in normal and Doppler-free configurations. The pressure broadening coefficients determined were {γ{{\\text{O}2}}}   =  0.40  ±  0.08  cm-1/bar for oxygen molecules and {γ\\text{He}}   =  0.46  ±  0.03 cm-1/bar for helium atoms. These correspond to pressure broadening rate constants k\\text{PB}{{\\text{O}2}}   =  9 · 10-9 cm3 s-1 and k\\text{PB}\\text{He}   =  4 · 10-9 cm3 s-1, respectively. The well-known quenching rate constants of O(3p 3 P J ) by O2 and He are at least one order of magnitude smaller, which signifies that non-quenching collisions constitute the main line-broadening mechanism. In addition to providing new insights into collisional processes of oxygen atoms in electronically excited 3p 3 P J state, reported pressure broadening parameters are important for quantification of oxygen TALIF line profiles when both collisional and Doppler broadening mechanisms are important. Thus, the Doppler component (and hence the temperature of oxygen atoms) can be accurately determined from high resolution TALIF measurements in a broad range of conditions.

  4. Real-Time Near-Field Terahertz Imaging with Atomic Optical Fluorescence

    CERN Document Server

    Wade, Christopher G; de Melo, Natalia R; Kondo, Jorge M; Adams, Charles S; Weatherill, Kevin J

    2016-01-01

    Terahertz (THz) near-field imaging is a flourishing discipline [1], with applications from fundamental studies of beam propagation [2,3] to the characterisation of metameterials [4,5] and waveguides [6,7]. Beating the diffraction limit typically involves rastering structures or detectors with length scale shorter than the radiation wavelength; in the THz domain this has been achieved using a number of techniques including scattering tips [8,9] and apertures [10]. Alternatively, mapping THz fields onto an optical wavelength and imaging the visible light removes the requirement for scanning a local probe, speeding up image collection times [11,12]. Here we report THz to optical conversion using a gas of highly excited `Rydberg' atoms. By collecting THz-induced optical fluorescence we demonstrate a real-time image of a THz standing wave and we use well-known atomic properties to calibrate the THz field strength. The mono-atomic gas does not distort the THz field and offers the potential to immerse structures wit...

  5. Semiconductor Nanomaterials-Based Fluorescence Spectroscopic and Matrix-Assisted Laser Desorption/Ionization (MALDI Mass Spectrometric Approaches to Proteome Analysis

    Directory of Open Access Journals (Sweden)

    Suresh Kumar Kailasa

    2013-12-01

    Full Text Available Semiconductor quantum dots (QDs or nanoparticles (NPs exhibit very unusual physico-chemcial and optical properties. This review article introduces the applications of semiconductor nanomaterials (NMs in fluorescence spectroscopy and matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS for biomolecule analysis. Due to their unique physico-chemical and optical properties, semiconductors NMs have created many new platforms for investigating biomolecular structures and information in modern biology. These semiconductor NMs served as effective fluorescent probes for sensing proteins and cells and acted as affinity or concentrating probes for enriching peptides, proteins and bacteria proteins prior to MALDI-MS analysis.

  6. 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

  7. A novel fluorescence "on-off-on" chemosensor for Hg(2+)via a water-assistant blocking heavy atom effect.

    Science.gov (United States)

    Wu, Chong; Zhao, Jiang-Lin; Jiang, Xue-Kai; Wang, Chuan-Zeng; Ni, Xin-Long; Zeng, Xi; Redshaw, Carl; Yamato, Takehiko

    2016-10-14

    Upper rim pyrene-functionalized hexahomotrioxacalix[3]arene L was synthesized via Click chemistry, and its fluorescence behaviors toward several common metal cations were investigated. L exhibited a significant fluorescence quenching response to Hg(2+) in CH3CN solution, which was unaffected by the coexistence of other competitive metal cations. Thus, L can be utilized as a highly selective and sensitive fluorescent chemosensor for Hg(2+) with a detection limit in the nM level. Interestingly, the quenched fluorescence emission can be successfully revived upon the addition of water. In this process, the heavy atom effect of Hg(2+) can be blocked by further coordination of a water molecule and resulted in the revival of the fluorescence emission of L/Hg(2+) complex. Particularly, other polar solvents such as CH3OH and CH3CH2OH also have the ability to revive the fluorescence emission of the L/Hg(2+) complex, but on a much smaller scale than observed for H2O. The heavy atom effect and blocking thereof were demonstrated within the same system by the use of a C3-symmetric homooxacalix[3]arene scaffold. The present studies provided further evidence for the blocking heavy atom effect.

  8. Speciation analysis of mercury in sediments, zoobenthos and river water samples by high-performance liquid chromatography hyphenated to atomic fluorescence spectrometry following preconcentration by solid phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Margetinova, Jana; Houserova-Pelcova, Pavlina [Department of Chemistry and Biochemistry, Mendel University of Agriculture and Forestry, Zemedelska 1, Brno CZ 613 00 (Czech Republic); Kuban, Vlastimil [Department of Chemistry and Biochemistry, Mendel University of Agriculture and Forestry, Zemedelska 1, Brno CZ 613 00 (Czech Republic)], E-mail: kuban@mendelu.cz

    2008-05-19

    A high-pressure microwave digestion was applied for microwave-assisted extraction (MAE) of mercury species from sediments and zoobenthos samples. A mixture containing 3 mol L{sup -1} HCl, 50% aqueous methanol and 0.2 mol L{sup -1} citric acid (for masking co-extracted Fe{sup 3+}) was selected as the most suitable extraction agent. The efficiency of proposed extraction method was better than 95% with R.S.D. below 6%. A preconcentration method utilizing a 'homemade' C18 solid phase extraction (SPE) microcolumns was developed to enhance sensitivity of the mercury species determination using on-column complex formation of mercury-2-mercaptophenol complexes. Methanol was chosen for counter-current elution of the retained mercury complexes achieving a preconcentration factor as much as 1000. The preconcentration method was applied for the speciation analysis of mercury in river water samples. The high-performance liquid chromatography-cold vapour atomic fluorescence spectrometric (HPLC/CV-AFS) method was used for the speciation analysis of mercury. The complete separation of four mercury species was achieved by an isocratic elution of aqueous methanol (65%/35%) on a Zorbax SB-C18 column (4.6 mm x 150 mm, 5 {mu}m) using the same complexation reagent (2-mercaptophenol). The limits of detection were 4.3 {mu}g L{sup -1} for methylmercury (MeHg{sup +}), 1.4 {mu}g L{sup -1} for ethylmercury (EtHg{sup +}), 0.8 {mu}g L{sup -1} for inorganic mercury (Hg{sup 2+}), 0.8 {mu}g L{sup -1} for phenylmercury (PhHg{sup +})

  9. Photoluminescence Enhancement in Nanotextured Fluorescent SiC Passivated by Atomic Layer Deposited Al2O3 Films

    DEFF Research Database (Denmark)

    Lu, Weifang; Ou, Yiyu; Jokubavicius, Valdas

    2016-01-01

    The influence of thickness of atomic layer deposited Al2O3 films on nano-textured fluorescent 6H-SiC passivation is investigated. The passivation effect on the light emission has been characterized by photoluminescence and time-resolved photoluminescence at room temperature. The results show that...

  10. Electrochemical hydride generation atomic fluorescence spectrometry for detection of tin in canned foods using polyaniline-modified lead cathode

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Xianjuan [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Gan Wuer, E-mail: wgan@ustc.edu.cn [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China); Wan Lingzhong; Deng Yun; Yang Qinghua; He Youzhao [Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026 (China)

    2010-12-15

    An electrochemical hydride generation system with polyaniline-modified lead cathode was developed for tin determination by coupling with atomic fluorescence spectrometry. The tin fluorescence signal intensity was improved evidently as the polyaniline membrane could facilitate the transformation process from atomic tin to the SnH{sub 4} and prevent the aggradation of Sn atom on Pb electrode surface. The effects of experimental parameters and interferences have been studied. The limit of detection (LOD) was 1.5 ng mL{sup -1} (3{sigma}) and the relative standard deviation (RSD) was 3.3% for 11 consecutive measurements of 50 ng mL{sup -1} Sn(IV) standard solution.

  11. On-line study of flavonoids of Trollius chinensis Bunge binding to DNA with ethidium bromide using a novel combination of chromatographic, mass spectrometric and fluorescence techniques.

    Science.gov (United States)

    Song, Zhiling; Wang, Hong; Ren, Biao; Zhang, Baobao; Hashi, Yuki; Chen, Shizhong

    2013-03-22

    The study of the interaction between drugs and DNA is an important way to understand the role of drug molecules. A novel online analytical method for this purpose combining high-performance liquid chromatography-diode array detector-electrospray ionization-ion-trap time-of-flight mass spectrometry (HPLC-DAD-ESI-IT-TOF-MS(n)) and DNA-ethidium bromide detection with a fluorescence detector (DNA-EB-FLD) was firstly developed, which could rapidly identify the chemical constituents and obtain the profile related to DNA binding activity. This method has been applied for a precise or probable identification of the chemical constituents by ultraviolet (UV) absorption and MS(n) data analysis, while the DNA binding profile has been characterized by directly measuring the fluorescence intensity of compound-DNA-EB. Using this method, Trollius chinensis Bunge was studied and 18 constituents were identified by MS(n) data; six of them (4'-methoxy-2″-O-(2‴-methylbutyryl)vitexin,2″-O-(3‴-methoxycaffeoyl)vitexin) and 4'-methoxy-2″-O-(2‴-methylbutyryl)orientin,acacetin-7-O-rutinoside,quercetin-3-O-xylosylglucoside,quercetin-3-O-arabinosylglucoside) were identified for the first time in T. chinensis Bunge, and 16 constituents accounted for its activity of binding to DNA. The established (HPLC-DAD-ESI-IT-TOF-MS(n) DNA-EB-FLD) system has proved to offer a useful strategy for correlating the chemical profile with the binding to DNA activities of the components without their isolation and purification, and may be used for multicomponent analysis of active substances in other herbs.

  12. 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

  13. Comparative biotransformation and disposition studies of nabumetone in humans and minipigs using high-performance liquid chromatography with ultraviolet, fluorescence and mass spectrometric detection.

    Science.gov (United States)

    Nobilis, M; Kopecký, J; Kvetina, J; Svoboda, Z; Pour, M; Kunes, J; Holcapek, M; Kolárová, L

    2003-08-08

    The disposition of the non-steroidal anti-inflammatory drug (NSAID) nabumetone after a single oral dose administration of nabumetone tablets to humans and minipigs was investigated. Nabumetone is a prodrug, which is metabolized in the organism to the principal pharmacodynamically active metabolite -- 6-methoxy-2-naphthylacetic acid (6-MNA), and some other minor metabolites (carbonyl group reduction products, O-desmethylation products and their conjugates with glucuronic and sulphuric acids). Standards of the above-mentioned metabolites were prepared using simple synthetic procedures and their structures were confirmed by NMR and mass spectrometry. A simple HPLC method for the simultaneous determination of nabumetone, 6-MNA and the other metabolites was developed, validated and used for xenobiochemical and pharmacokinetic studies in humans and minipigs and for distribution studies in minipigs. Naproxen was chosen as the internal standard (I.S.), both UV (for higher concentrations) and fluorescence detection (for very low concentrations) were used. The identity of the nabumetone metabolites in biological samples was confirmed using HPLC-MS experiments. Pharmacokinetics of nabumetone, 6-MNA and 6-HNA (6-hydroxy-2-naphthylacetic acid) in human and minipig plasma was evaluated and compared. The concentration levels of nabumetone metabolites in urine, bile and synovial fluid were also evaluated.

  14. 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.)

  15. [Research on optimization of mathematical model of flow injection-hydride generation-atomic fluorescence spectrometry].

    Science.gov (United States)

    Cui, Jian; Zhao, Xue-Hong; Wang, Yan; Xiao, Ya-Bing; Jiang, Xue-Hui; Dai, Li

    2014-01-01

    Flow injection-hydride generation-atomic fluorescence spectrometry was a widely used method in the industries of health, environmental, geological and metallurgical fields for the merit of high sensitivity, wide measurement range and fast analytical speed. However, optimization of this method was too difficult as there exist so many parameters affecting the sensitivity and broadening. Generally, the optimal conditions were sought through several experiments. The present paper proposed a mathematical model between the parameters and sensitivity/broadening coefficients using the law of conservation of mass according to the characteristics of hydride chemical reaction and the composition of the system, which was proved to be accurate as comparing the theoretical simulation and experimental results through the test of arsanilic acid standard solution. Finally, this paper has put a relation map between the parameters and sensitivity/broadening coefficients, and summarized that GLS volume, carrier solution flow rate and sample loop volume were the most factors affecting sensitivity and broadening coefficients. Optimizing these three factors with this relation map, the relative sensitivity was advanced by 2.9 times and relative broadening was reduced by 0.76 times. This model can provide a theoretical guidance for the optimization of the experimental conditions.

  16. Elasticity Maps of Living Neurons Measured by Combined Fluorescence and Atomic Force Microscopy

    CERN Document Server

    Spedden, Elise; Naumova, Elena N; Kaplan, David L; Staii, Cristian

    2013-01-01

    Detailed knowledge of mechanical parameters such as cell elasticity, stiffness of the growth substrate, or traction stresses generated during axonal extensions is essential for understanding the mechanisms that control neuronal growth. Here we combine Atomic Force Microscopy based force spectroscopy with Fluorescence Microscopy to produce systematic, high-resolution elasticity maps for three different types of live neuronal cells: cortical (embryonic rat), embryonic chick dorsal root ganglion, and P-19 (mouse embryonic carcinoma stem cells) neurons. We measure how the stiffness of neurons changes both during neurite outgrowth and upon disruption of microtubules of the cell. We find reversible local stiffening of the cell during growth, and show that the increase in local elastic modulus is primarily due to the formation of microtubules. We also report that cortical and P-19 neurons have similar elasticity maps, with elastic moduli in the range 0.1-2 kPa, with typical average values of 0.4 kPa (P-19) and 0.2 k...

  17. Determination of mercury in rice by cold vapor atomic fluorescence spectrometry after microwave-assisted digestion

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Maria Jose da [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Paim, Ana Paula S. [Departamento de Quimica Fundamental, Universidade Federal de Pernambuco, Cidade Universitaria, 50740-550 Recife, PE (Brazil); Pimentel, Maria Fernanda [Departamento de Engenharia Quimica, Universidade Federal de Pernambuco, Recife, PE (Brazil); Cervera, M. Luisa, E-mail: m.luisa.cervera@uv.es [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain); Guardia, Miguel de la [Department of Analytical Chemistry, Edificio de Investigacion, University of Valencia, 50 Dr. Moliner Street, E-46100 Burjassot, Valencia (Spain)

    2010-05-14

    A cold vapor atomic fluorescence spectrometry method (CV-AFS) has been developed for the determination of Hg in rice samples at a few ng g{sup -1} concentration level. The method is based on the previous digestion of samples in a microwave oven with HNO{sub 3} and H{sub 2}O{sub 2} followed by dilution with water containing KBr/KBrO{sub 3} and hydroxylamine and reduction with SnCl{sub 2} in HCl using external calibration. The matrix interferences and the effect of nitrogen oxide vapors have been evaluated and the method validated using a certified reference material. The limit of detection of the method was 0.9 ng g{sup -1} with a recovery percentage of 95 {+-} 4% at an added concentration of 5 ng g{sup -1}. The concentration level of Hg found in 24 natural rice samples from different origin ranged between 1.3 and 7.8 ng g{sup -1}.

  18. [Determination of mercury in shark liver by cold atom fluorescence spectrometry after microwave dissolution].

    Science.gov (United States)

    Weng, Di

    2005-12-01

    The conditions for the determination of mercury in shark liver by cold atom fluorescence spectrometry (CAFS) with microwave dissolution were studied. After being dried completely, the method employed 2 mol x L(-1) HNO3-4 mol x L(-1) HCl as an oxidant, and with catalysis by V2O5, the samples were digested in a microwave oven. The mercury in absorption solution was reduced by SnCl2, and then was determined by CAFS at wavelength of 253.7 nm. 10% SnCl2 solution was used as a reductive agent for mercury. The linear range was 0-2.0 ng x mL(-1) mercury (r = 0.999 7). The detection limit was 0.05 ng x mL(-1), the relative standard deviation was 0.86%-2.22%, and the average recovery rate was 96.0%-108.5%. The method was suitable for the determination of mercury in shark liver.

  19. Novel Method for Indirect Determination of Iodine in Marine Products by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    LU Jian-ping; TAN Fang-wei; TANG Qiong; JIANG Tian-cheng

    2013-01-01

    A method for the determination of iodine based upon compound H2HgI4,formed between I-and Hg2+ in nitric acid and extracted in methyl isobutyl ketone(MIBK),was developed via atomic fluorescence spectrometry(AFS).After the compound is reduced with potassium borohydrid(KBH4),the resultant mercury vapor was injected into the instrument and iodine was,therefore,indirectly determined.Experimental parameters such as the conditions of extraction reagents,aqueous phase acidity,elemental mercury diffusion temperature in a vial and other factors were investigated and optimized.Under the optimum experimental conditions,this method shows a detection limit of 0.038 μg/L iodine and a linear relationship between 0.04-20 μg/L.The method was applied to determining the iodine content in marine duck eggs,kelps,laver and Ganoderma lucidum spirulina,showing a relative standard deviation(RSD) of 2.15% and the recoveries in the range of 98.1%-102.5%.

  20. Determination of Arsenic in Matricaria chamomilla L.by microwave digestion-atomic fluorescence spectrometry%微波消解-原子荧光光谱法测定洋甘菊中砷的含量

    Institute of Scientific and Technical Information of China (English)

    辛禄德; 李强; 王建玲; 劳斐; 田树革

    2014-01-01

    Objective To develop an atomic fluorescence spectrometric method for the determination of Ar-senic in Matricaria chamomilla L.Methods Sample was digested with microwave digestion system.The Arsenic was directly analyzed by atomic fluorescence spectrometry,and the methodology of the study was investigated.Results The content of arsenic within the range of 0-10.0 μg/L the correlative coefficient of the calibration curves was over 0.999 3,the average recovery was 100.81% with RSD of 2.59% (n =6). Conclusion The method is convenient,stable,less harmful and highly sensitive.%目的:建立洋甘菊中砷含量的原子荧光光谱检测方法。方法采用微波消解样品,通过原子荧光光谱法测定洋甘菊中砷含量,并进行了方法学考察。结果砷在0~10.0μg/L (r =0.9993)范围内峰面积与浓度呈良好线性关系,平均加样回收率为100.81%,RSD=2.59%(n =6)。结论该测量方法简便、稳定、危害小、灵敏度高。

  1. Laser-induced atomic fragment fluorescence spectroscopy: a facile technique for molecular spectroscopy of spin-forbidden states.

    Science.gov (United States)

    Zhang, Qun; Chen, Yang; Keil, Mark

    2009-03-01

    Spectra of spin-forbidden and spin-allowed transitions in the mixed b (3)Pi(u) approximately A (1)Sigma(u)(+) state of Na(2) are measured separately by two-photon excitation using a single tunable dye laser. The two-photon excitation produces Na(*)(3p) by photodissociation, which is easily and sensitively detected by atomic fluorescence. At low laser power, only the A (1)Sigma(u)(+) state is excited, completely free of triplet excitation. At high laser power, photodissociation via the intermediate b (3)Pi(u) triplet state becomes much more likely, effectively "switching" the observations from singlet spectroscopy to triplet spectroscopy with only minor apparatus changes. This technique of perturbation-assisted laser-induced atomic fragment fluorescence may therefore be especially useful as a general vehicle for investigating perturbation-related physics pertinent to the spin-forbidden states, as well as for studying allowed and forbidden states of other molecules.

  2. 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.

  3. 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.

  4. Characterization of national food agency shrimp and plaice reference materials for trace elements and arsenic species by atomic and mass spectrometric techniques

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pedersen, Gitte Alsing; McLaren, J. W.

    1997-01-01

    , drying, milling and sieving to collect the fraction of particles less than 150 mu m in sizer In this fraction the trace elements were homogeneously distributed using a 400 mg sample intake for analysis, The total track element concentrations were determined by graphite furnace and cold vapour atomic...... absorption spectrometry, inductively coupled plasma mass spectrometry (ICP-MS) and isotope dilution ICP-MS. The contents of arsenobetaine and the tetramethylarsonium ion were determined by cation exchange high performance liquid chromatography (HPLC) coupled with ICP-MS, or coupled with ion-spray (IS) tandem...... mass spectrometry (MS/MS) for qualitative verification, Based on a rigorous statistical analysis of the analytical data using the DANREF software, it was decided to assign certified values for mercury, cadmium and arsenic in the NFA Shrimp, and mercury, selenium and arsenic in the NFA Plaice...

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

    Science.gov (United States)

    Tsogas, George Z; Giokas, Dimosthenis L; Vlessidis, Athanasios G

    2009-04-30

    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 microg L(-1) for Cd(2+), 0.05-0.10 microg L(-1) for Pb(2+) and 0.1-0.25 microg L(-1) for Sn(4+) 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.

  6. Potential of two-line atomic fluorescence for temperature imaging in turbulent indium-oxide-producing flames

    Energy Technology Data Exchange (ETDEWEB)

    Münsterjohann, Bettina; Huber, Franz J. T.; Klima, Tobias C.; Holfelder, Sandra; Engel, Sascha R. [Friedrich-Alexander Universität Erlangen-Nürnberg (FAU), Lehrstuhl für Technische Thermodynamik (LTT) (Germany); Miller, Joseph D. [Aerospace Systems Directorate, Air Force Research Laboratory (United States); Meyer, Terrence R. [Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU), Erlangen Graduate School in Advanced Optical Technologies (SAOT) (Germany); Will, Stefan, E-mail: stefan.will@fau.de [Friedrich-Alexander Universität Erlangen-Nürnberg (FAU), Lehrstuhl für Technische Thermodynamik (LTT) (Germany)

    2015-11-15

    The applicability of two-line atomic fluorescence (TLAF) for temperature imaging in an indium-based flame spray pyrolysis (FSP) process is demonstrated using a single tunable optical parametric oscillator (OPO) to generate the required excitation wavelengths consecutively. Single-shot images of the detected fluorescence signals demonstrate that the signal levels in the flame are suitable for evaluation of temperature and verify the capability and potential of the measurement technique directly during particle formation without additional indium seeding. Qualitative averaged two-dimensional temperature distributions in the FSP flame are presented, showing the influence of varying sheath gas flow rates on the resulting temperature distribution. With the addition of a second OPO and detection system, the two fluorescence signals acquired consecutively in this work could be obtained simultaneously and enable spatio-temporally resolved single-shot temperature measurements in flame synthesis processes of indium-containing nanoparticles.

  7. Correlative atomic force and confocal fluorescence microscopy: single molecule imaging and force induced spectral shifts (Conference Presentation)

    Science.gov (United States)

    Basché, Thomas; Hinze, Gerald; Stöttinger, Sven

    2016-09-01

    A grand challenge in nanoscience is to correlate structure or morphology of individual nano-sized objects with their photo-physical properties. An early example have been measurements of the emission spectra and polarization of single semiconductor quantum dots as well as their crystallographic structure by a combination of confocal fluorescence microscopy and transmission electron microscopy.[1] Recently, the simultaneous use of confocal fluorescence and atomic force microscopy (AFM) has allowed for correlating the morphology/conformation of individual nanoparticle oligomers or molecules with their photo-physics.[2, 3] In particular, we have employed the tip of an AFM cantilever to apply compressive stress to single molecules adsorbed on a surface and follow the effect of the impact on the electronic states of the molecule by fluorescence spectroscopy.[3] Quantum mechanical calculations corroborate that the spectral changes induced by the localized force can be associated to transitions among the different possible conformers of the adsorbed molecule.

  8. 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.

  9. Column preconcentration of gold by adsorbing AuCl4- onto methyltrioctyl ammonium chloride-naphthalene and subsequent atomic absorption spectrometric determination.

    Science.gov (United States)

    Behpour, M; Attaran, A M; Ghoreishi, S M; Soltani, N

    2005-05-01

    A sensitive, selective and simple preconcentration method for ultra-trace gold determination has been developed that uses naphthalene-methyltrioctyl ammonium chloride (Aliquat 336s) as an adsorbent. Gold, in the form of AuCl4-, was retained by the adsorbent in the column at a flow rate of 1 ml min(-1). After filtration, the solid mass consisting of the gold complex and naphthalene was dissolved out of the column with 5 ml of N,N-dimethylformamide (DMF), and the metal was then determined by atomic absorption spectrometry. In the initial solution, the calibration graph of absorbance versus gold concentration was found to be linear in the range 0.5-150 ng ml(-1) Au(III) with r=0.997 (n=9), and the 3 s detection limit was 0.428 ng ml(-1). The relative standard deviation for eight replicate measurements of 20 microg of gold was 2.14%. Preconcentration factors of 390 and 650 were achieved using 5 ml and 3 ml of DMF, respectively. The proposed method was successfully applied to the determination of gold in wastewater, processed pool water, slurry pool water, and raw well-water from the Moteh gold mine, and synthetic samples.

  10. The study of applicability of dithiocarbamate-coated fullerene C 60 for preconcentration of palladium for graphite furnace atomic absorption spectrometric determination in environmental samples

    Science.gov (United States)

    Leśniewska, Barbara A.; Godlewska, Iwona; Godlewska—Żyłkiewicz, Beata

    2005-03-01

    The present method comprises an off-line enrichment of Pd on the fullerene, C 60, coated with ammonium pyrrolidinedithiocarbamate (APDC), followed by the elution of formed Pd-chelate with ethanol and the subsequent determination of Pd from the eluate by graphite furnace atomic absorption spectrometry. By using fullerene loaded with 0.1% APDC, the analytical system is simplified as the sample can be directly preconcentrated on the column. The following parameters affecting the preconcentration of Pd on C 60 were optimized: amount of ligand used for the coating of fullerene, sample pH, kind of eluent, sample and eluent flow rates, volume and number of fractions of eluent used. The sorption efficiency for Pd on coated fullerene was 99.2±1.1%. The best elution efficiency for Pd from the column was obtained with 0.6 ml of ethanol at a flow rate of 0.2 ml min -1. The limit of detection was 0.044 ng ml -1. The effect of sample pretreatment procedure on the preconcentration of Pd by evaluated method is discussed. The content of Pd in road dust (179.2±17.4 ng g -1) determined by proposed method was in agreement with the results obtained with a reference method. The low recovery of analyte (64%) was obtained for geological material CRM SARM-7 (platinum ore) due to the much higher concentration of interfering elements.

  11. The study of applicability of dithiocarbamate-coated fullerene C{sub 60} for preconcentration of palladium for graphite furnace atomic absorption spectrometric determination in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Lesniewska, Barbara A. [Institute of Chemistry, University of BiaIystok, Hurtowa 1, 15-399 BiaIystok (Poland); Godlewska, Iwona [Institute of Chemistry, University of BiaIystok, Hurtowa 1, 15-399 BiaIystok (Poland); GodlewskayIkiewicz, Beata [Institute of Chemistry, University of BiaIystok, Hurtowa 1, 15-399 BiaIystok (Poland)]. E-mail: bgodlew@uwb.edu.pl

    2005-03-31

    The present method comprises an off-line enrichment of Pd on the fullerene, C{sub 60}, coated with ammonium pyrrolidinedithiocarbamate (APDC), followed by the elution of formed Pd-chelate with ethanol and the subsequent determination of Pd from the eluate by graphite furnace atomic absorption spectrometry. By using fullerene loaded with 0.1% APDC, the analytical system is simplified as the sample can be directly preconcentrated on the column. The following parameters affecting the preconcentration of Pd on C{sub 60} were optimized: amount of ligand used for the coating of fullerene, sample pH, kind of eluent, sample and eluent flow rates, volume and number of fractions of eluent used. The sorption efficiency for Pd on coated fullerene was 99.2{+-}1.1%. The best elution efficiency for Pd from the column was obtained with 0.6 ml of ethanol at a flow rate of 0.2 ml min{sup -1}. The limit of detection was 0.044 ng ml{sup -1}. The effect of sample pretreatment procedure on the preconcentration of Pd by evaluated method is discussed. The content of Pd in road dust (179.2{+-}17.4 ng g{sup -1}) determined by proposed method was in agreement with the results obtained with a reference method. The low recovery of analyte (64%) was obtained for geological material CRM SARM-7 (platinum ore) due to the much higher concentration of interfering elements.

  12. 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.

  13. 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.

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

    Science.gov (United States)

    Ghaedi, Mehrorang; Shokrollahi, Ardeshir; Niknam, Khodabakhsh; Niknam, Ebrahim; Najibi, Asma; Soylak, Mustafa

    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 1molL(-1) HNO(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(-1) for Cd(2+), Pb(2+), Pd(2+) and Ag(+) along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd(2+), Pb(2+), Pd(2+) 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.

  15. 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.

  16. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Energy Technology Data Exchange (ETDEWEB)

    Angeli, Valeria [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Biagi, Simona [National Research Council of Italy, C.N.R., Istituto per i Processi Chimico-Fisici - IPCF-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Ghimenti, Silvia [University of Pisa, Department of Chemistry and Industrial Chemistry, Via Risorgimento 35, 56126 Pisa (Italy); Onor, Massimo; D' Ulivo, Alessandro [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Bramanti, Emilia, E-mail: bramanti@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici - ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2011-11-15

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H{sub 2} miniaturized flame after sodium borohydride reduction to Hg{sup 0}, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H{sub 2} microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10{sup -5} mol L{sup -1}), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L{sup -1} (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 {mu}mol L{sup -1} were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were

  17. Flow injection-chemical vapor generation atomic fluorescence spectrometry hyphenated system for organic mercury determination: A step forward

    Science.gov (United States)

    Angeli, Valeria; Biagi, Simona; Ghimenti, Silvia; Onor, Massimo; D'Ulivo, Alessandro; Bramanti, Emilia

    2011-11-01

    Monomethylmercury and ethylmercury were determined on line using flow injection-chemical vapor generation atomic fluorescence spectrometry without neither requiring a pre-treatment with chemical oxidants, nor UV/MW additional post column interface, nor organic solvents, nor complexing agents, such as cysteine. Inorganic mercury, monomethylmercury and ethylmercury were detected by atomic fluorescence spectrometry in an Ar/H 2 miniaturized flame after sodium borohydride reduction to Hg 0, monomethylmercury hydride and ethylmercury hydride, respectively. The effect of mercury complexing agent such as cysteine, ethylendiaminotetracetic acid and HCl with respect to water and Ar/H 2 microflame was investigated. The behavior of inorganic mercury, monomethylmercury and ethylmercury and their cysteine-complexes was also studied by continuous flow-chemical vapor generation atomic fluorescence spectrometry in order to characterize the reduction reaction with tetrahydroborate. When complexed with cysteine, inorganic mercury, monomethylmercury and ethylmercury cannot be separately quantified varying tetrahydroborate concentration due to a lack of selectivity, and their speciation requires a pre-separation stage (e.g. a chromatographic separation). If not complexed with cysteine, monomethylmercury and ethylmercury cannot be separated, as well, but their sum can be quantified separately with respect to inorganic mercury choosing a suitable concentration of tetrahydroborate (e.g. 10 - 5 mol L - 1 ), thus allowing the organic/inorganic mercury speciation. The detection limits of the flow injection-chemical vapor generation atomic fluorescence spectrometry method were about 45 nmol L - 1 (as mercury) for all the species considered, a relative standard deviation ranging between 1.8 and 2.9% and a linear dynamic range between 0.1 and 5 μmol L - 1 were obtained. Recoveries of monomethylmercury and ethylmercury with respect to inorganic mercury were never less than 91%. Flow injection

  18. Collective resonance fluorescence in small and dense atom clouds: Comparison between theory and experiment

    CERN Document Server

    Jenkins, S D; Javanainen, J; Jennewein, S; Bourgain, R; Pellegrino, J; Sortais, Y R P; Browaeys, A

    2016-01-01

    We study the emergence of a collective optical response of a cold and dense $^{87}$Rb atomic cloud to a near-resonant low-intensity light when the atom number is gradually increased. Experimental observations are compared with microscopic stochastic simulations of recurrent scattering processes between the atoms that incorporate the atomic multilevel structure and the optical measurement setup. We analyze the optical response of an inhomogeneously-broadened gas and find that the experimental observations of the resonance line shifts and the total collected scattered light intensity in cold atom clouds substantially deviate from those of thermal atomic ensembles, indicating strong light-induced resonant dipole-dipole interactions between the atoms. At high densities, the simulations also predict a significantly slower decay of light-induced excitations in cold than in thermal atom clouds. The role of dipole-dipole interactions is discussed in terms of resonant coupling examples and the collective radiative exc...

  19. 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.

  20. 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.

  1. New Homogeneous Standards by Atomic Layer Deposition for Synchrotron X-ray Fluorescence and Absorption Spectroscopies.

    Energy Technology Data Exchange (ETDEWEB)

    Butterworth, A.L.; Becker, N.; Gainsforth, Z.; Lanzirotti, A.; Newville, M.; Proslier, T.; Stodolna, J.; Sutton, S.; Tyliszczak, T.; Westphal, A.J.; Zasadzinski, J. (UCB)

    2012-03-13

    Quantification of synchrotron XRF analyses is typically done through comparisons with measurements on the NIST SRM 1832/1833 thin film standards. Unfortunately, these standards are inhomogeneous on small scales at the tens of percent level. We are synthesizing new homogeneous multilayer standards using the Atomic Layer Deposition technique and characterizing them using multiple analytical methods, including ellipsometry, Rutherford Back Scattering at Evans Analytical, Synchrotron X-ray Fluorescence (SXRF) at Advanced Photon Source (APS) Beamline 13-ID, Synchrotron X-ray Absorption Spectroscopy (XAS) at Advanced Light Source (ALS) Beamlines 11.0.2 and 5.3.2.1 and by electron microscopy techniques. Our motivation for developing much-needed cross-calibration of synchrotron techniques is borne from coordinated analyses of particles captured in the aerogel of the NASA Stardust Interstellar Dust Collector (SIDC). The Stardust Interstellar Dust Preliminary Examination (ISPE) team have characterized three sub-nanogram, {approx}1{micro}m-sized fragments considered as candidates to be the first contemporary interstellar dust ever collected, based on their chemistries and trajectories. The candidates were analyzed in small wedges of aerogel in which they were extracted from the larger collector, using high sensitivity, high spatial resolution >3 keV synchrotron x-ray fluorescence spectroscopy (SXRF) and <2 keV synchrotron x-ray transmission microscopy (STXM) during Stardust ISPE. The ISPE synchrotron techniques have complementary capabilities. Hard X-ray SXRF is sensitive to sub-fg mass of elements Z {ge} 20 (calcium) and has a spatial resolution as low as 90nm. X-ray Diffraction data were collected simultaneously with SXRF data. Soft X-ray STXM at ALS beamline 11.0.2 can detect fg-mass of most elements, including cosmochemically important oxygen, magnesium, aluminum and silicon, which are invisible to SXRF in this application. ALS beamline 11.0.2 has spatial resolution

  2. Atoms

    Institute of Scientific and Technical Information of China (English)

    刘洪毓

    2007-01-01

    Atoms(原子)are all around us.They are something like the bricks (砖块)of which everything is made. The size of an atom is very,very small.In just one grain of salt are held millions of atoms. Atoms are very important.The way one object acts depends on what

  3. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Energy Technology Data Exchange (ETDEWEB)

    Liu Qingyang, E-mail: liuqingyang0807@yahoo.com.c [Beijing Center for Physical and Chemical Analysis, Beijing 100089 (China)

    2010-07-15

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg{sup 0}, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL{sup -1} for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury (n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

  4. Direct determination of mercury in white vinegar by matrix assisted photochemical vapor generation atomic fluorescence spectrometry detection

    Science.gov (United States)

    Liu, Qingyang

    2010-07-01

    This paper proposes the use of photochemical vapor generation with acetic acid as sample introduction for the direct determination of ultra-trace mercury in white vinegars by atomic fluorescence spectrometry. Under ultraviolet irradiation, the sample matrix (acetic acid) can reduce mercury ion to atomic mercury Hg 0, which is swept by argon gas into an atomic fluorescence spectrometer for subsequent analytical measurements. The effects of several factors such as the concentration of acetic acid, irradiation time, the flow rate of the carrier gas and matrix effects were discussed and optimized to give detection limits of 0.08 ng mL -1 for mercury. Using the experimental conditions established during the optimization (3% v/v acetic acid, 30 s irradiation time and 20 W mercury lamp), the precision levels, expressed as relative standard deviation, were 4.6% (one day) and 7.8% (inter-day) for mercury ( n = 9). Addition/recovery tests for evaluation of the accuracy were in the range of 92-98% for mercury. The method was also validated by analysis of vinegar samples without detectable amount of Hg spiked with aqueous standard reference materials (GBW(E) 080392 and GBW(E) 080393). The results were also compared with those obtained by acid digestion procedure and determination of mercury by ICP-MS. There was no significant difference between the results obtained by the two methods based on a t-test (at 95% confidence level).

  5. Photolytic-interference-free, femtosecond, two-photon laser-induced fluorescence imaging of atomic oxygen in flames

    Science.gov (United States)

    Kulatilaka, Waruna D.; Roy, Sukesh; Jiang, Naibo; Gord, James R.

    2016-02-01

    Ultrashort-pulse lasers are well suited for nonlinear diagnostic techniques such as two-photon laser-induced fluorescence (TPLIF) because the signals generated scale as the laser intensity squared. Furthermore, the broad spectral bandwidths associated with nearly Fourier-transform-limited ultrashort pulses effectively contribute to efficient nonlinear excitation by coupling through a large number of in-phase photon pairs, thereby producing strong fluorescence signals. Additionally, femtosecond (fs)-duration amplified laser systems typically operate at 1-10 kHz repetition rates, enabling high-repetition-rate imaging in dynamic environments. In previous experiments, we have demonstrated utilization of fs pulses for kilohertz (kHz)-rate, interference-free imaging of atomic hydrogen (H) in flames. In the present study, we investigate the utilization of fs-duration pulses to photolytic-interference-free TPLIF imaging of atomic oxygen (O). In TPLIF of O, photodissociation of vibrationally excited carbon dioxide (CO2) is known to be the prominent interference that produces additional O atoms in the medium. We have found that through the use of fs excitation, such interferences can be virtually eliminated in premixed laminar methane flames, which paves the way for two-dimensional imaging of O at kHz data rates. Such measurements can provide critical data for validating complex, multidimensional turbulent-combustion models as well as for investigating flame dynamics in practical combustion devices.

  6. 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.

  7. Laser-Excited Atomic Fluorescence and Ionization in a Graphite Furnace for the Determination of Metals and Nonmetals

    Science.gov (United States)

    Butcher, David James

    1990-01-01

    Here is reported novel instrumentation for atomic spectrometry that combined the use of a pulsed laser system as the light source and an electrothermal atomizer as the atom cell. The main goal of the research was to develop instrumentation that was more sensitive for elemental analysis than commercially available instruments and could be used to determine elements in real sample matrices. Laser excited atomic fluorescence spectrometry (LEAFS) in an electrothermal atomizer (ETA) was compared to ETA atomic absorption spectrometry (AAS) for the determination of thallium, manganese, and lead in food and agricultural standard reference materials (SRMs). Compared to ETA AAS, ETA LEAFS has a longer linear dynamic range (LDR) (5-7 orders of magnitude compared to 2-3 orders of magnitude) and higher sensitivity (10 ^{-16} to 10^{ -14} g as compared to 10^{ -13} to 10^{-11} g). Consequently, ETA LEAFS allows elemental analysis to be done over a wider range of concentrations with less dilution steps. Thallium was accurately determined in biological samples by ETA LEAFS at amounts five to one hundred times below the ETA AAS detection limit. ETA AAS and ETA LEAFS were compared for the determination of lead and manganese, and in general, the accuracies and precisions of ETA AAS were the same, with typical precisions between 3% and 6%. Fluorine was determined using laser excited molecular fluorescence spectrometry (LEMOFS) in an ETA. Molecular fluorescence from magnesium fluoride was collected, and the detection limit of 0.3 pg fluorine was two to six orders of magnitude more sensitive than other methods commonly used for the determination of fluorine. Significant interferences from ions were observed, but the sensitivity was high enough that fluorine could be determined in freeze dried urine SRMs by diluting the samples by a factor of one hundred to remove the interferences. Laser enhanced ionization (LEI) in an ETA was used for the determination of metals. For thallium, indium

  8. Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

    Science.gov (United States)

    Cizdziel, James V.

    2011-01-01

    In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

  9. Total uncertainty budget calculation for the determination of mercury in incineration ash (BCR 176R) by atomic fluorescence spectrometry.

    Science.gov (United States)

    Tirez, Kristof; Beutels, Filip; Brusten, Wilfried; Noten, Bart; De Brucker, Nicole

    2002-11-01

    The mercury mass fraction has been determined by atomic fluorescence spectrometry (AFS) in the framework of the project "Certification of a reference material (trace elements in fly ash) in replacement of BCR CRM 176". Calculation of the uncertainty budget, as described in this manuscript, emphasizes a practical and realistic approach to estimation of uncertainty components on the basis of statistical assumptions. GUM Workbench software was used, and resulted in a mercury mass fraction of 1.58+/-0.11 mg kg(-1) (with coverage factor k=2.2, 95% probability) related to dry mass, submitted in the certification exercise. The calculated total uncertainty budget applies to analogous samples analyzed by this procedure.

  10. Spatially and Temporally Resolved Atomic Oxygen Measurements in Short Pulse Discharges by Two Photon Laser Induced Fluorescence

    Science.gov (United States)

    Lempert, Walter; Uddi, Mruthunjaya; Mintusov, Eugene; Jiang, Naibo; Adamovich, Igor

    2007-10-01

    Two Photon Laser Induced Fluorescence (TALIF) is used to measure time-dependent absolute oxygen atom concentrations in O2/He, O2/N2, and CH4/air plasmas produced with a 20 nanosecond duration, 20 kV pulsed discharge at 10 Hz repetition rate. Xenon calibrated spectra show that a single discharge pulse creates initial oxygen dissociation fraction of ˜0.0005 for air like mixtures at 40-60 torr total pressure. Peak O atom concentration is a factor of approximately two lower in fuel lean (φ=0.5) methane/air mixtures. In helium buffer, the initially formed atomic oxygen decays monotonically, with decay time consistent with formation of ozone. In all nitrogen containing mixtures, atomic oxygen concentrations are found to initially increase, for time scales on the order of 10-100 microseconds, due presumably to additional O2 dissociation caused by collisions with electronically excited nitrogen. Further evidence of the role of metastable N2 is demonstrated from time-dependent N2 2^nd Positive and NO Gamma band emission spectroscopy. Comparisons with modeling predictions show qualitative, but not quantitative, agreement with the experimental data.

  11. 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...

  12. Speciation analysis of arsenic by selective hydride generation-cryotrapping-atomic fluorescence spectrometry with flame-in-gas-shield atomizer: achieving extremely low detection limits with inexpensive instrumentation.

    Science.gov (United States)

    Musil, Stanislav; Matoušek, Tomáš; Currier, Jenna M; Stýblo, Miroslav; Dědina, Jiří

    2014-10-21

    This work describes the method of a selective hydride generation-cryotrapping (HG-CT) coupled to an extremely sensitive but simple in-house assembled and designed atomic fluorescence spectrometry (AFS) instrument for determination of toxicologically important As species. Here, an advanced flame-in-gas-shield atomizer (FIGS) was interfaced to HG-CT and its performance was compared to a standard miniature diffusion flame (MDF) atomizer. A significant improvement both in sensitivity and baseline noise was found that was reflected in improved (4 times) limits of detection (LODs). The yielded LODs with the FIGS atomizer were 0.44, 0.74, 0.15, 0.17 and 0.67 ng L(-1) for arsenite, total inorganic, mono-, dimethylated As and trimethylarsine oxide, respectively. Moreover, the sensitivities with FIGS and MDF were equal for all As species, allowing for the possibility of single species standardization with arsenate standard for accurate quantification of all other As species. The accuracy of HG-CT-AFS with FIGS was verified by speciation analysis in two samples of bottled drinking water and certified reference materials, NRC CASS-5 (nearshore seawater) and SLRS-5 (river water) that contain traces of methylated As species. As speciation was in agreement with results previously reported and sums of all quantified species corresponded with the certified total As. The feasibility of HG-CT-AFS with FIGS was also demonstrated by the speciation analysis in microsamples of exfoliated bladder epithelial cells isolated from human urine. The results for the sums of trivalent and pentavalent As species corresponded well with the reference results obtained by HG-CT-ICPMS (inductively coupled plasma mass spectrometry).

  13. Simultaneous Laser-induced Fluorescence of Nitric Oxide and Atomic Oxygen in the Hypersonic Materials Environment Test System Arcjet Facility

    Science.gov (United States)

    Johansen, Craig; Lincoln, Daniel; Bathel, Brett; Inman, Jennifer; Danehy, Paul

    2014-01-01

    Simultaneous nitric oxide (NO) and atomic oxygen (O) laser induced fluorescence (LIF) experiments were performed in the Hypersonic Materials Environmental Test System (HYMETS) facility at the NASA Langley Research Center. The data serves as an experimental database for validation for chemical and thermal nonequilibrium models used in hypersonic flows. Measurements were taken over a wide range of stagnation enthalpies (6.7 - 18.5 MJ/kg) using an Earth atmosphere simulant with a composition of 75% N2, 20% O2, and 5% Ar (by volume). These are the first simultaneous measurements of NO and O LIF to be reported in literature for the HYMETS facility. The maximum O LIF mean signal intensity was observed at a stagnation enthalpy of approximately 12 MJ/kg while the maximum NO LIF mean signal intensity was observed at a stagnation enthalpy of 6.7 MJ/kg. Experimental results were compared to simple fluorescence model that assumes equilibrium conditions in the plenum and frozen chemistry in the isentropic nozzle expansion (Mach 5). The equilibrium calculations were performed using CANTERA v2.1.1 with 16 species. The fluorescence model captured the correlation in mean O and NO LIF signal intensities over the entire range of stagnation enthalpies tested. Very weak correlations between single-shot O and NO LIF intensities were observed in the experiments at all of the stagnation enthalpy conditions.

  14. Synchronizing atomic force microscopy force mode and fluorescence microscopy in real time for immune cell stimulation and activation studies

    Energy Technology Data Exchange (ETDEWEB)

    Cazaux, Séverine; Sadoun, Anaïs; Biarnes-Pelicot, Martine; Martinez, Manuel; Obeid, Sameh [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France); Bongrand, Pierre [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France); APHM, Hôpital de la Conception, Laboratoire d’Immunologie, Marseille F-13385 (France); Limozin, Laurent [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France); Puech, Pierre-Henri, E-mail: pierre-henri.puech@inserm.fr [Aix Marseille Université, LAI UM 61, Marseille F-13288 (France); Inserm, UMR-S 1067, Marseille F-13288 (France); CNRS, UMR 7333, Marseille F-13288 (France)

    2016-01-15

    A method is presented for combining atomic force microscopy (AFM) force mode and fluorescence microscopy in order to (a) mechanically stimulate immune cells while recording the subsequent activation under the form of calcium pulses, and (b) observe the mechanical response of a cell upon photoactivation of a small G protein, namely Rac. Using commercial set-ups and a robust signal coupling the fluorescence excitation light and the cantilever bending, the applied force and activation signals were very easily synchronized. This approach allows to control the entire mechanical history of a single cell up to its activation and response down to a few hundreds of milliseconds, and can be extended with very minimal adaptations to other cellular systems where mechanotransduction is studied, using either purely mechanical stimuli or via a surface bound specific ligand. - Highlights: • A signal coupling AFM and fluorescence microscopy was characterized for soft cantilevers. • It can be used as an intrinsic timer to synchronize images and forces. • Mechanical stimulation of single immune cells while recording calcium fluxes was detailed. • Light-induced mechanical modifications of lymphocytes using a PA-Rac protein were demonstrated. • The precautions and limitations of use of this effect were presented.

  15. Determination of cadmium in rice and water by tungsten coil electrothermal vaporization-atomic fluorescence spectrometry and tungsten coil electrothermal atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Wen Xiaodong [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Wu Peng [Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Chen Li [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Hou Xiandeng, E-mail: houxd@scu.edu.cn [College of Chemistry, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China); Analytical and Testing Center, Sichuan University, 29 Wangjiang Road, Chengdu, Sichuan 610064 (China)

    2009-09-14

    In this work, the microsampling nature of tungsten coil electrothermal vaporization Ar/H{sub 2} flame atomic fluorescence spectrometry (W-coil ETV-AFS) as well as tungsten coil electrothermal atomic absorption spectrometry (W-coil ET-AAS) was used with cloud point extraction (CPE) for the ultrasensitive determination of cadmium in rice and water samples. When the temperature of the extraction system is higher than the cloud point temperature of the selected surfactant Triton X-114, the complex of cadmium with dithizone can be quantitatively extracted into the surfactant-rich phase and subsequently separated from the bulk aqueous phase by centrifugation. The main factors affecting the CPE, such as concentration of Triton X-114 and dithizone, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimal conditions, the limits of detection for cadmium by W-coil ETV-AFS and W-coil ET-AAS were 0.01 and 0.03 {mu}g L{sup -1}, with sensitivity enhancement factors of 152 and 93, respectively. The proposed methods were applied to the determination of cadmium in certified reference rice and water samples with analytical results in good agreement with certified values.

  16. Statistics of resonance fluorescence of a pair of atoms in a feedback loop

    Energy Technology Data Exchange (ETDEWEB)

    Tomilin, V. A., E-mail: 8342tomilin@mail.ru; Il' ichev, L. V. [Russian Academy of Sciences, Institute of Automatics and Electrometry, Siberian Branch (Russian Federation)

    2013-02-15

    The statistics of photoemission events of a pair of closely spaced two-level atoms is calculated in a classical light field whose phase is changed by {pi} after the detection of each spontaneous photon. This statistics is compared with the statistics in the case when the feedback is missing. In both cases, one can observe noticeable antibunching of photons in the range of parameters where no antibunching is observed in a single-atom system. The feedback substantially increases the antibunching. This effect manifests itself more strongly in relatively weak fields and for considerable frequency detunings.

  17. Computer simulations on resonant fluorescence spectra in atomic gases in two monochromatic laser fields of arbitrary intensity and magnetic field

    Science.gov (United States)

    Karagodova, Tamara Y.

    1996-03-01

    In the intense radiation fields with power density from 104W/cm2 to 109W/cm2 the essential modification of electronic states of atoms occurs displaying, in particular, in modifications of resonant fluorescence (rf) spectra. We use 'Fermi golden rule' for calculations of relative intensities and frequencies for rf multiplet for real multilevel initially unexcited atoms in two monochromatic laser fields of arbitrary intensity resonant to adjacent transitions of (Xi) or (Lambda) types and magnetic field, giving the level splittings of different values from Zeeman to Paschen-Back effect. The dependence of quasienergies on parameters obtained with the help of a sorting program permits us to define the values of parameters for which the states of the system are mixed and so to receive the correct probability amplitudes for instantaneous or adiabatic regimes of switching the perturbation. The analysis of the quasienergies and form of rf spectra permits us to get relations between the form of the spectra and modifications of electronic structure of the atom due to radiation fields and external magnetic field.

  18. Imaging magnetic scalar potentials by laser-induced fluorescence from bright and dark atoms

    CERN Document Server

    Fescenko, Ilja

    2014-01-01

    We present a spectroscopic method for mapping two-dimensional distributions of magnetic field strengths (magnetic scalar potential lines) using CCD recordings of the fluorescence patterns emitted by spin-polarized Cs vapor in a buffer gas exposed to inhomogeneous magnetic fields. The method relies on the position-selective destruction of spin polarization by magnetic resonances induced by multi-component oscillating magnetic fields, such that magnetic potential lines can directly be detected by the CCD camera. We also present a generic algebraic model allowing the calculation of the fluorescence patterns and find excellent agreement with the experimental observations for three distinct inhomogeneous field topologies. The spatial resolution obtained with these proof-of-principle experiments is on the order of 1 mm. A substantial increase of spatial and magnetic field resolution is expected by deploying the method in a magnetically shielded environment.

  19. Improving the analytical performance of hydride generation non-dispersive atomic fluorescence spectrometry. Combined effect of additives and optical filters

    Science.gov (United States)

    D'Ulivo, Alessandro; Bramanti, Emilia; Lampugnani, Leonardo; Zamboni, Roberto

    2001-10-01

    The effects of tetrahydroborate and acid concentration and the presence of L-cysteine and thiourea were investigated in the determination of As, Bi and Sn using continuous flow hydride generation atomic fluorescence spectrometry (HG AFS). The aim was to find conditions allowing the control of those effects exerting negative influence on the analytical performance of the HG AFS apparatus. The effects taken into account were: (i) the radiation scattering generated by carryover of solution from the gas-liquid separator to the atomizer; (ii) the introduction of molecular species generated by tetrahydroborate decomposition into the atomizer; and (iii) interference effects arising from other elements in the sample matrix and from different acids. The effects (i) and (ii) could be controlled using mild reaction conditions in the HG stage. The effect of HG conditions on carryover was studied by radiation scattering experiments without hydride atomization. Compromised HG conditions were found by studying the effects of tetrahydroborate (0.1-20 g l -1) and acid (0.01-7 mol l -1) concentration, and the addition of L-cysteine (10 g l -1) and thiourea (0.1 mol l -1) on the HG AFS signals. The effect of optical filters was investigated with the aim of improving the signal-to-noise ratio. Optical filters with peak wavelengths of 190 and 220 nm provided an improvement of detection limits by factors of approximately 4 and 2 for As and Te, respectively. Under optimized conditions the detection limits were 6, 5, 3, 2, 2 and 9 ng l -1 for As, Sb, Bi, Sn, Se and Te, respectively. Good tolerance to various acid compositions and sample matrices was obtained by using L-cysteine or thiourea as masking agents. Determination of arsenic in sediment and copper certified reference materials, and of bismuth in steel, sediment, soil and ore certified reference material is reported.

  20. Development of the spectrometric imaging apparatus of laser induced fluorescence from plants and estimation of chlorophyll contents of rice leaves; Laser reiki keiko sokutei sochi no kaihatsu to inehanai no chlorophyll ganryo no suitei

    Energy Technology Data Exchange (ETDEWEB)

    Nakaya, K.; Shoji, K.; Hanyu, H.

    1999-05-01

    Photosynthetic activity of plants is an important factor to assess the micrometeorological effect of plant canopy or to estimate the influence of circumstances such as water stress. Light illumination induces fluorescence from a leaf or suspension of chloroplasts. The red chlorophyll fluorescence had been used to determine the process of the electron transportation in photosynthetic reaction. The fluorescence source other than chlorophyll is not announced sufficiently, but is supposed to be useful to determine the contents of the substance corresponding to physiological response of plants. We developed a fluorescence imaging apparatus to observe spectrum and distribution of laser induced fluorescence from a leaf. Pulsed UV-laser (Nd:YAG) induced blue-green fluorescence and red chlorophyll fluorescence from a green leaf. The pulse modulated measuring light and CCD with image-intensifier (ICCD) enable to detect the fluorescence from plants under illumination. The laser induced fluorescence (LIF) spectra were investigated to estimate the chlorophyll contents in leaves of rice. During the greening course of dark grown etiolated rice leaves, chlorophyll contents were determined using the extraction of leaves and steady state LIF spectra were measured. As a result, the ratio of fluorescent intensity between blue-green and red peaks (F460/F740 and F510/F740) decreased in proportion to alteration of chlorophyll contents respectively. These fluorescence intensity ratios perform more precise estimation of higher chlorophyll contents of leaves than reported red chlorophyll fluorescence intensity ratio (F690/E740). (author)

  1. 原子荧光光谱法测定土壤中的砷含量%Determination of Arsenic in Soil by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘燕芬

    2015-01-01

    通过结合具体的试验对运用原子荧光光谱法测定土壤中的砷含量进行了探讨,以期能为有关方面的需要提供有益的参考和借鉴。%In order to provide a useful reference for the relevant aspects of the arsenic content in soil by atomic fluorescence spectrometry, the method of atomic fluorescence spectrometry was used to determine the arsenic content in soil.

  2. Silver atom and strand numbers in fluorescent and dark Ag:DNAs.

    Science.gov (United States)

    Schultz, Danielle; Gwinn, Elisabeth G

    2012-06-11

    We use tandem HPLC-mass spectrometry with in-line spectroscopy to identify silver atom numbers, N(Ag), of 10 to 21 in visible- to infrared-emitting Ag:DNA complexes stabilized by oligonucleotide monomers and dimers. Qualitatively different absorbance spectra from bare, same-N(Ag) silver clusters point to silver-base interactions as the origin for the color of Ag:DNAs.

  3. Pentavalent antimony uptake pathway through erythrocyte membranes: molecular and atomic fluorescence approaches.

    Science.gov (United States)

    Barrera, Camila; López, Silvana; Aguilar, Luis; Mercado, Luis; Bravo, Manuel; Quiroz, Waldo

    2016-04-01

    Previous studies by our group have shown that Sb(V) is able to enter red blood cells in a dynamic process and is reduced to Sb(III) by glutathione. The present study aims to investigate a possible entry pathway for Sb(V) through the erythrocyte membrane. Applying fluorescence spectroscopy studies with Laurdan and diphenylhexatriene (DPH) probes, it was found that there was no interaction between Sb(V) and membrane lipids. By comparing the Sb(V) entry percentages through lipid vesicles and sealed erythrocyte membranes, it was found that Sb(V) required protein channels to pass through the membrane. The competitive inhibition results using HCO3 (-) and Cl(-) showed that the Sb(V) uptake rate through the membrane fell approximately 50-70 % until full inhibition was reached, which was possibly due to the inhibition of the anion exchanger 1 (AE1) channel. Finally, the fluorescence measurements with the 5-iodoacetamidofluorescein (5-IAF) probe showed that Sb(V) interacted with membrane protein SH groups during this process.

  4. A new way towards high-efficiency thermally activated delayed fluorescence devices via external heavy-atom effect

    Science.gov (United States)

    Zhang, Wenzhi; Jin, Jiangjiang; Huang, Zhi; Zhuang, Shaoqing; Wang, Lei

    2016-07-01

    Thermally activated delayed fluorescence (TADF) mechanism is a significant method that enables the harvesting of both triplet and singlet excitons for emission. However, up to now most efforts have been devoted to dealing with the relation between singlet-triplet splitting (ΔEST) and fluorescence efficiency, while the significance of spin-orbit coupling (SOC) is usually ignored. In this contribution, a new method is developed to realize high-efficiency TADF-based devices through simple device-structure optimizations. By inserting an ultrathin external heavy-atom (EHA) perturber layer in a desired manner, it provides useful means of accelerating the T1 → S1 reverse intersystem crossing (RISC) in TADF molecules without affecting the corresponding S1 → T1 process heavily. Furthermore, this strategy also promotes the utilization of host triplets through Förster mechanism during host → guest energy transfer (ET) processes, which helps to get rid of the solely dependence upon Dexter mechanism. Based on this strategy, we have successfully raised the external quantum efficiency (EQE) in 4CzPN-based devices by nearly 38% in comparison to control devices. These findings provide keen insights into the role of EHA played in TADF-based devices, offering valuable guidelines for utilizing certain TADF dyes which possess high radiative transition rate but relatively inefficient RISC.

  5. Atomic force microscopy for analyzing metaphase chromosomes: comparison of AFM images with fluorescence labeling images of banding patterns.

    Science.gov (United States)

    Hoshi, Osamu; Ushiki, Tatsuo

    2014-01-01

    The combined use of fluorescence microscopy with atomic force microscopy (AFM) has been introduced to analyze the replication-banding patterns of human chromosomes. Human lymphocytes synchronized with excess thymidine are treated with 5-ethynyl-2'-deoxyuridine (EdU) during the late S phase. EdU-labeled DNA is detected in metaphase chromosomes using Alexa Fluor 488(®) azide, through the 1,3-dipolar cycloaddition reaction of organic azides with the terminal acetylene group of EdU. Chromosomes with EdU incorporated during the late S phase show a banding pattern similar to the G-banding pattern of normal human chromosomes. The comparison between the fluorescence and AFM image of the same chromosome indicates the presence of ridges and grooves in the chromatid arms, which correspond to G-positive and G-negative bands, respectively. This technique of EdU-labeled replication bands combined with AFM is useful to analyze the structure of chromosomes in relation to the banding pattern.

  6. Production mechanism of atomic nitrogen in atmospheric pressure pulsed corona discharge measured using two-photon absorption laser-induced fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Teramoto, Yoshiyuki; Ono, Ryo [Department of Advanced Energy, University of Tokyo, 5-1-5 Kashiwanoha, Kashiwa, Chiba 227-8568 (Japan); Oda, Tetsuji [Department of Electrical Engineering, University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656 (Japan)

    2012-06-01

    To study the production mechanism of atomic nitrogen, the temporal profile and spatial distribution of atomic nitrogen are measured in atmospheric pressure pulsed positive corona discharge using two-photon absorption laser-induced fluorescence. The absolute atomic nitrogen density in the streamer filaments is estimated from decay rate of atomic nitrogen in N{sub 2} discharge. The results indicate that the absolute atomic nitrogen density is approximately constant against discharge energy. When the discharge voltage is 21.5 kV, production yield of atomic nitrogen produced by an N{sub 2} discharge pulse is estimated to be 2.9 - 9.8 Multiplication-Sign 10{sup 13} atoms and the energy efficiency of atomic nitrogen production is estimated to be about 1.8 - 6.1 Multiplication-Sign 10{sup 16} atoms/J. The energy efficiency of atomic nitrogen production in N{sub 2} discharge is constant against the discharge energy, while that in N{sub 2}/O{sub 2} discharge increases with discharge energy. In the N{sub 2}/O{sub 2} discharge, two-step process of N{sub 2} dissociation plays significant role for atomic nitrogen production.

  7. Determination of lead in wine by hydride generation atomic fluorescence spectrometry in the presence of hexacyanoferrate(III).

    Science.gov (United States)

    Karadjova, Irina B; Lampugnani, Leonardo; D'Ulivo, Alessandro; Onor, Massimo; Tsalev, Dimiter L

    2007-06-01

    A rapid, accurate, and precise method is described for the determination of Pb in wine using continuous-flow hydride generation atomic fluorescence spectrometry (CF-HGAFS). Sample pretreatment consists of ten-fold dilution of wine followed by direct plumbane generation in the presence of 0.1 mol L(-1) HCl and 1% m/v K(3)[Fe(CN)(6)] with 1% m/v NaBH(4) as reducing agent. An aqueous standard calibration curve is recommended for Pb quantification in wine sample. The method provides a limit of detection and a limit of quantification of 0.3 microg L(-1) and 1 microg L(-1), respectively. The relative standard deviation varies between 2-6% (within-run) and 4-11% (between-run) at 3-30 microg L(-1) Pb levels in wine. Good agreement has been demonstrated between results obtained by CF-HGAFS and direct electrothermal atomic absorption spectrometry in analyses of red and white wines within the concentration range of 9.2-25.8 microg L(-1) Pb.

  8. Atomically precise arrays of fluorescent silver clusters: a modular approach for metal cluster photonics on DNA nanostructures.

    Science.gov (United States)

    Copp, Stacy M; Schultz, Danielle E; Swasey, Steven; Gwinn, Elisabeth G

    2015-03-24

    The remarkable precision that DNA scaffolds provide for arraying nanoscale optical elements enables optical phenomena that arise from interactions of metal nanoparticles, dye molecules, and quantum dots placed at nanoscale separations. However, control of ensemble optical properties has been limited by the difficulty of achieving uniform particle sizes and shapes. Ligand-stabilized metal clusters offer a route to atomically precise arrays that combine desirable attributes of both metals and molecules. Exploiting the unique advantages of the cluster regime requires techniques to realize controlled nanoscale placement of select cluster structures. Here we show that atomically monodisperse arrays of fluorescent, DNA-stabilized silver clusters can be realized on a prototypical scaffold, a DNA nanotube, with attachment sites separated by <10 nm. Cluster attachment is mediated by designed DNA linkers that enable isolation of specific clusters prior to assembly on nanotubes and preserve cluster structure and spectral purity after assembly. The modularity of this approach generalizes to silver clusters of diverse sizes and DNA scaffolds of many types. Thus, these silver cluster nano-optical elements, which themselves have colors selected by their particular DNA templating oligomer, bring unique dimensions of control and flexibility to the rapidly expanding field of nano-optics.

  9. Rocket observation of atomic oxygen and night airglow: Measurement of concentration with an improved resonance fluorescence technique

    Directory of Open Access Journals (Sweden)

    K. Kita

    Full Text Available An improved resonant fluorescence instrument for measuring atomic oxygen concentration was developed to avoid the Doppler effect and the aerodynamic shock effect due to the supersonic motion of a rocket. The shock effect is reduced by adopting a sharp wedge-shaped housing and by scanning of the detector field of view to change the distance between the scattering volume and the surface of the housing. The scanning enables us to determine absolute values of atomic oxygen concentration from relative variation of the scattered light signal due to the self-absorption. The instrument was calibrated in the laboratory, and the numerical simulation reproduced the calibration result. Using the instrument, the altitude profile of atomic oxygen concentration was observed by a rocket experiment at Uchinoura (31°N on 28 January 1992. The data obtained from the rocket experiment were not perfectly free from the shock effect, but errors due to the effect were reduced by the data analysis procedure. The observed maximum concentration was 3.8× 1011 cm–3 at altitudes around 94 km. The systematic error is estimated to be less than ±0.7×1011 cm–3 and the relative random error is less than±0.07× 1011 cm–3at the same altitudes. The altitude profile of the OI 557.7-nm airglow was also observed in the same rocket experiment. The maximum volume emission rate was found to be 150 photons cm–3 s–1 at 94 km. The observed altitude profiles are compared with the MSIS model and other in situ observations.

  10. Dielectric barrier discharges with steep voltage rise: mapping of atomic nitrogen in single filaments measured by laser-induced fluorescence spectroscopy

    Science.gov (United States)

    Lukas, C.; Spaan, M.; Schulz-von der Gathen, V.; Thomson, M.; Wegst, R.; Döbele, H. F.; Neiger, M.

    2001-08-01

    Space and time resolved relative atomic density distributions of nitrogen have been measured for the first time at a single filament within a dielectric barrier discharge (DBD) reactor with submillimetre radial dimensions. Two-photon-Absorption Laser-Induced Fluorescence (TALIF) spectroscopy of atomic nitrogen using radiation at λ = 206.7 nm is applied to a DBD with fast rising voltage amplitudes. The decay time of the atomic nitrogen density depends strongly on the position within the discharge and the distance from the dielectric where the lifetime is maximum. Admixed oxygen leads to an increase of the N density decay by an order of magnitude even at small fractions.

  11. An expression for the atomic fluorescence and thermal-emission intensity under conditions of near saturation and arbitrary self-absorption

    NARCIS (Netherlands)

    Omenetto, N.; Winefordner, J.D.; Alkemade, C.T.J.

    1975-01-01

    An expression for the effect of self-absorption on the fluorescence and thermal emission intensities is derived by taking into account stimulated emission. A simple, idealized case is considered, consisting of a two level atomic system, in a flame, homogeneous with respect to temperature and composi

  12. Measurement of total angular momentum values of high-lying even-parity atomic states of samarium by spectrally resolved laser-induced fluorescence technique

    Indian Academy of Sciences (India)

    A K Pulhani; M L Shah; G P Gupta; B M Suri

    2010-12-01

    Spectrally resolved laser-induced fluorescence technique was used to uniquely assign total angular momentum () values to high-lying even-parity energy levels of atomic samarium. Unique value assignment was done for seven energy levels in the energy region 34,800–36,200 cm-1 , recently observed and reported in the literature.

  13. Ambient-temperature trap/release of arsenic by dielectric barrier discharge and its application to ultratrace arsenic determination in surface water followed by atomic fluorescence spectrometry

    Science.gov (United States)

    A novel dielectric barrier discharge reactor (DBDR) was utilized to trap/release arsenic coupled to hydride generation atomic fluorescence spectrometry (HGAFS). On the DBD principle, the precise and accurate control of trap/release procedures was fulfilled at ambient temperature, and an analytical m...

  14. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Science.gov (United States)

    Li, Shan; Wang, Mei; Zhong, Yizhou; Zhang, Zehua; Yang, Bingyi

    2015-09-01

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea-ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries.

  15. Two-photon absorption laser induced fluorescence measurement of atomic oxygen density in an air atmospheric pressure plasma jet

    Science.gov (United States)

    Conway, Jim; Gogna, Gurusharan; Daniels, Stephen

    2016-09-01

    Two-photon Absorption Laser Induced Fluorescence (TALIF) is used to measure atomic oxygen number density [O] in an air Atmospheric Pressure Plasma Jet (APPJ). A novel technique based on photolysis of O2 is used to calibrate the TALIF system ensuring the same species (O) is probed during calibration and measurement. As a result, laser intensity can be increased outside the TALIF quadratic laser power region without affecting calibration reliability as any high intensity saturation effects will be identical for calibration and experiment. Higher laser intensity gives stronger TALIF signals helping overcome weak TALIF signals often experienced at atmospheric pressure due to collisional quenching. O2 photo-dissociation and two-photon excitation of the resulting [O] are both achieved within the same laser pulse. The photolysis [O] is spatially non-uniform and time varying. To allow valid comparison with [O] in a plasma, spatial and temporal correction factors are required. Knowledge of the laser pulse intensity I0(t), and wavelength allows correction factors to be found using a rate equation model. The air flow into the jet was fixed and the RF power coupled into the system varied. The resulting [O] was found to increase with RF power.

  16. Determination of arsenic speciation in sulfidic waters by Ion Chromatography Hydride-Generation Atomic Fluorescence Spectrometry (IC-HG-AFS).

    Science.gov (United States)

    Keller, Nicole S; Stefánsson, Andri; Sigfússon, Bergur

    2014-10-01

    A method for the analysis of arsenic species in aqueous sulfide samples is presented. The method uses an ion chromatography system connected with a Hydride-Generation Atomic Fluorescence Spectrometer (IC-HG-AFS). With this method inorganic As(III) and As(V) species in water samples can be analyzed, including arsenite (HnAs(III)O3(n-3)), thioarsenite (HnAs(III)S3(n-3)), arsenate (HnAs(V)O4(n-3)), monothioarsenate (HnAs(V)SO3(n-3)), dithioarsenate (HnAs(V)S2O2(n-3)), trithioarsenate (HnAs(V)S3O(n-3)) and tetrathioarsenate (HnAs(V)S4(n-3)). The peak identification and retention times were determined based on standard analysis of the various arsenic compounds. The analytical detection limit was ~1-3 µg L(-1) (LOD), depending on the quality of the baseline. This low detection limit makes this method also applicable to discriminate between waters meeting the drinking water standard of max. 10 µg L(-1) As, and waters that do not meet this standard. The new method was successfully applied for on-site determination of arsenic species in natural sulfidic waters, in which seven species were unambiguously identified.

  17. Determination of lead in environmental waters with dispersive liquid-liquid microextraction prior to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Qingxiang, E-mail: zhouqx@cup.edu.cn [School of Chemistry and Environmental Sciences, Henan Normal University, Henan Key Laboratory for Environmental Pollution Control, Key Laboratory for Yellow River and Huaihe River Water Environment and Pollution Control, Ministry of Education, Xinxiang 453007 (China); State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Zhao, Na [State Laboratory of Petroleum Resource and Prospecting, College of Geosciences, China University of Petroleum Beijing, Beijing 102249 (China); Xie, Guohong [College of Resources and Environment, Henan Institute of Science and Technology, Xinxiang 453003 (China)

    2011-05-15

    This paper established a new, rapid and sensitive method for the determination of lead in water samples preconcentrated by dispersive liquid-liquid microextraction (DLLME) prior to atomic fluorescence spectrometry. Dithizone was used as the chelating agent. In the DLLME procedure, lead formed lead-dithizone complex and migrated into the carbon tetrachloride micro-droplets. Important factors that would affect the extraction efficiency had been investigated including the kind and volume of extraction solvent and dispersive solvent, sample pH, the amount of chelating agent, extraction time and centrifugation time. The results showed that the coexisting ions containing in water samples had no obvious negative effect on the determination of lead. The experimental results indicated that the proposed method had a good linear range of 0.01-100 ng mL{sup -1} (r{sup 2} = 0.9990). The precision was 2.12% (RSD, n = 7) and the detection limit was 0.95 ng L{sup -1}. Proposed method was validated with four real environmental samples and the results indicated that the proposed method was excellent for the future use and satisfied spiked recoveries were in the range of 92.9-97.4%.

  18. Development of an analytical method for antimony speciation in vegetables by HPLC-hydride generation-atomic fluorescence spectrometry.

    Science.gov (United States)

    Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea; Neaman, Alexander; Quiroz, Waldo

    2012-01-01

    A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 microg/L and 5.0, 5.2, and 4.7%, respectively, for a 100 microL sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts.

  19. Antimony speciation analysis in sediment reference materials using high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Potin-Gautier, M. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Pannier, F. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France)]. E-mail: Florence.pannier@univ-pau.fr; Quiroz, W. [Laboratoire de Chimie Analytique, BioInorganique et Environnement LCABIE (UMR CNRS 3054), Universite de Pau et des pays de l' Adour, 64000 Pau (France); Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Pinochet, H. [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile); Gregori, I. de [Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Pontificia Universidad catolica de Valparaiso (Chile)

    2005-11-30

    This work presents the development of suitable methodologies for determination of the speciation of antimony in sediment reference samples. Liquid chromatography with a post-column photo-oxidation step and hydride generation atomic fluorescence spectrometry as detection system is applied to the separation and determination of Sb(III), Sb(V) and trimethylantimony species. Post-column decomposition and hydride generation steps were studied for sensitive detection with the AFS detector. This method was applied to investigate the conditions under which speciation analysis of antimony in sediment samples can be carried out. Stability studies of Sb species during the extraction processes of solid matrices, using different reagents solutions, were performed. Results demonstrate that for the extraction yield and the stability of Sb species in different marine sediment extracts, citric acid in ascorbic acid medium was the best extracting solution for antimony speciation analysis in this matrix (between 55% and 65% of total Sb was recovered from CRMs, Sb(III) being the predominant species). The developed method allows the separation of the three compounds within 6 min with detection limits of 30 ng g{sup -1} for Sb(III) and TMSbCl2 and 40 ng g{sup -1} for Sb(V) in sediment samples.

  20. In situ Determination of Anthracene Adsorbed onto Mangrove Root Surface Micro-zone Using Microscopic Fluorescence Spectrometric Analysis System%显微荧光光谱原位测定红树植物根表面微区中的蒽

    Institute of Scientific and Technical Information of China (English)

    谭华东; 李锐龙; 朱亚先; 张勇

    2016-01-01

    A microscopic fluorescence spectrometric analysis ( MFSA) system was set in the laboratory. A novel method for in situ determination of Anthracene ( Ant) adsorbed onto root surface micro-zone of two kinks of mangrove plant, named Kandelia obovata ( K. obovata) and Avicennia marina ( A. marina) by MFSA was established. Fluorescence spectra of Ant adsorbed on root surface micro-zone were obtained by synchronous scanning mode. The signal to noise (S/N) of Ant (5. 3 pg/μm2) adsorbed on K. obovata and A. marina root surface micro-zone increased up to 5. 5 and 6. 8 while wavelength offset (△λ) both were at 60 nm, respectively. The linear dynamic ranges of established method were 5. 3-63. 2 pg/μm2 for K. obovata and 10. 5-52. 6 pg/μm2 for A. marina, with the detection limits of 1. 1 pg/μm2 and 5. 5 pg/μm2 , respectively. The relative standard deviations were both less than 12 . 5% ( n=9 ) , and the recoveries were 98 . 1% -117. 0% and 81. 2%-110. 9%, respectively. The result showed that the MFSA system had ability to obtain quantitative information of fluorescence spectra and fluorescence image of Ant adsorbed onto plant roots surface micro-zone.%自行搭建显微荧光光谱分析( Microscopic fluorescence spectrometric analysis, MFSA)系统,并将其用于吸附于红树植物秋茄( Kandelia obovata, K. obovata)和白骨壤( Avicennia marina, A. marina)根表面微区中蒽( Anthrancene, Ant)的原位测定。在同步扫描模式下,以波长差为60 nm,吸附于K. obovata和A. marina根表面微区中Ant(5.3 pg/μm2)的荧光信号有最大信噪比(5.5和6.8)。所建方法的线性范围分别为5.3 ~63.2 pg/μm2和10.5~52.6 pg/μm2,检出限分别为1.1和5.5 pg/μm2,相对标准偏差均小于12.5%(n=9),加标回收率分别为98.1%~117.0%和81.2%~110.9%。结果表明,搭建的MFSA系统具备原位获取植物根表面微区Ant荧光光谱定量信息和荧光图像信息的能力。

  1. Simultaneous determination of p-arsanilic acid and roxarsone in feed by liquid chromatography-hydride generation online coupled with atomic fluorescence spectrometry.

    Science.gov (United States)

    Liu, Jianjing; Yu, Hongxia; Song, Haibin; Qiu, Jing; Sun, Fengmei; Li, Ping; Yang, Shuming

    2008-08-01

    A novel, simple and sensitive liquid chromatography-hydride generation online coupled with atomic fluorescence spectrometry (LC-HG-AFS) method was developed for simultaneous determination of p-arsanilic acid (p-ASA) and roxarsone in feed. 20% Methanol aqueous was used as extraction reagent, after preprocessing samples by ultrasonic oscillation, then injected into the chromatography Waters symmetry shield RP18 analytical column (150mm x 4.6mm, 5 microm), finally detected by an atomic fluorescence spectrometer. The calibration curves of analyses were linear over a range of concentrations (0.2-4mg L-1 and the correlation coefficients were higher than 0.9990. The limits of detection were 0.2 mg L-1. The method has been validated by linearity, precision and recovery. p-ASA and roxarsone in feed can be successfully and simultaneously determined using the developed method without a tedious pretreatment procedure.

  2. Determination of trace selenium in high purity tellurium by hydride generation atomic fluorescence spectrometry after solid phase extraction of a diaminobenzidine-selenium chelate

    Science.gov (United States)

    Tong, Wang; Ying, Zeng; Jinyong, Xu

    2016-09-01

    Macroporous adsorption resin was used as the sorbent for solid phase extraction and determination of the trace Se content in high purity tellurium prior to hydride generation atomic fluorescence spectrometry analysis. Selenium was converted into an organic Se chelate using 3,3‧-diaminobenzidine and was separated from the tellurium matrix by solid phase extraction. The resin was packed as a column for solid phase extraction. Under optimum conditions, trace Se can be quantitatively extracted and the tellurium matrix can be removed. The Se in the eluate was determined by hydride generation atomic fluorescence spectrometry. The limit of detection (3σ) of this method was 0.22 ng g- 1 and the relative standard deviation (RSD, n = 5) ranged from 2.0 to 2.5% for the three investigated tellurium samples. The proposed method was successfully applied for the determination of the trace Se content in high purity tellurium samples.

  3. Matrix-assisted laser desorption/ionization time-of-flight and nano-electrospray ionization ion trap mass spectrometric characterization of 1-cyano-2-substituted-benz[f]isoindole derivatives of peptides for fluorescence detection

    DEFF Research Database (Denmark)

    Linnemayr, K; Brückner, A; Körner, R;

    1999-01-01

    A series of hexa- to decapeptides (molecular mass range 800-1200) were labeled with naphthalene-2,3-dicarboxaldehyde, which preferentially reacts with the primary amino groups of a peptide. A highly stable peptide conjugate is formed, which allows selective analysis by fluorescence at excitation...

  4. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shan, E-mail: ls_tuzi@163.com; Wang, Mei, E-mail: wmei02@163.com; Zhong, Yizhou, E-mail: yizhz@21cn.com; Zhang, Zehua, E-mail: kazuki.0101@aliyun.com; Yang, Bingyi, E-mail: e_yby@163.com

    2015-09-01

    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea–ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries. - Highlights: • Cloud point extraction was firstly established to determine trace inorganic arsenic(As) species combining with HGAFS. • Separate As(III) and As(V) determinations improve the accuracy. • Ultrasonic release of complexed As(V) enables complete As(V) reduction to As(III). • Direct HGAFS analysis can be performed.

  5. Polymorphism of Two-Dimensional Cyanine Dye J-Aggregates and Its Genesis: Fluorescence Microscopy and Atomic Force Microscopy Study.

    Science.gov (United States)

    Prokhorov, Valery V; Perelygina, Olga M; Pozin, Sergey I; Mal'tsev, Eugene I; Vannikov, Anatoly V

    2015-12-01

    Polymorphic J-aggregates of monomethine cyanine dye 3,3'-di(γ-sulfopropyl)-5,5'-dichlorotiamonomethinecyanine (TC) have been studied by fluorescence optical microscopy (FOM) and by atomic force microscopy (AFM). The in situ FOM observations in a solution drop distinguish two J-aggregate morphology classes: flexible strips and rigid rods. The AFM imaging of dried samples reveals a strong J-aggregate structural rearrangement under adsorption on a mica surface with the strips self-folding and the rods squashing into rectangular bilayers and much deeper destruction. In the present work, the following structural conclusions have been drawn on the basis of careful consideration of strip crystal habits and various structural features of squashed/destructed rods: (1) the tubular morphology of TC rods is directly proved by FOM measurements in the solution bulk; (2) the staircase model of molecular arrangement in strips is proposed explaining the characteristic ∼44° skew angle in strip vertices; (3) a model of tube formation by a close-packed helical winding of flexible monolayer strips is proposed and justified which explains the observed J-aggregate polymorphism and strip-to-rod polymorphic transformations in a wide spatiotemporal scale; (4) at a nanoscale, an unexpectedly complex quasi-one-dimensional organization in J-aggregate two-dimensional monolayers is observed by high-resolution AFM imaging of constituent nanostrips separated by a characteristic distance in the range of 6-10 nm. The obtained results indicate that the underlying monolayer structure is the same for all J-aggregate polymorphs.

  6. Continuous Determination of Heavy Metals in Water by Atomic Fluorescence and Atomic Absorption Spectrometry%原子荧光和原子吸收法连续测定水中的重金属

    Institute of Scientific and Technical Information of China (English)

    谢倩

    2015-01-01

    通过剖析原子荧光和原子吸收法的不同消解体系,优化实验条件,确定了原子荧光和原子吸收法连续测定水中的硒、砷、锌、铜的含量的最佳消解条件和最佳仪器测定条件。经加标回收以及标样分析,连续测定的灵敏度高,回收率在95.9%~109%之间,相对标准误差低于4.41%,操作简便快速,结果精确。%By analyzing the different digestion system of atomic fluorescence and atomic absorption method and optimizing experimental conditions, the optimal digestion conditions and the best measurement conditions of instruments for continuous determination selenium, arsenic, zinc, copper content in water by atomic fluorescence and atomic absorption spectrometry were determined.Spiking recovery and standard analysis result showed that continuous measurement had high sensitivity, and the recoveries was between 95.9% and 109%, relative standard deviation was less than 4.41%, the operation was simple, rapid and accurate.

  7. The estimation of the possibilities of synchrotron radiation X-ray fluorescent analysis and atomic specrometry for the bone's elemental composition determination

    Science.gov (United States)

    Gonchar, A. M.; Kolmogorov, U. P.; Gladkikh, E. A.; Shuvaeva, O. V.; Beisel, N. F.; Kolosova, N. G.

    2005-05-01

    Possibilities of multielemental highly sensitive techniques of analysis have been studied: synchrotron radiation X-ray fluorescence analysis (SR XFA), and atomic emission spectrometry with inductively bound plasma (ISP) and atomic absorption spectrometry (AAS) with flame (air-acetylene) atomization for assay of element composition of bone tissue with minimal preparation procedure. Results of comparative studies of elemental composition of bone tissue samples from experimental animals with inherited accelerated aging (rats of OXYS strain) using the SR XFA, ISP and AAS techniques are presented. It is shown that there exists in principle a possibility of assay of 22 biologically important essential macro- and trace elements within the range of 1.0-100,000 μg/g with a mean square analysis error of no more them 10-15% when using SR XFA.

  8. Determination of Inorganic Arsenic in Atmospheric Particles by Hydride Generation-atomic Fluorescence Spectrometry%氢化物发生-原子荧光光谱法测定大气颗粒物中的砷形态

    Institute of Scientific and Technical Information of China (English)

    梁淑轩; 吴虹; 齐学先; 郑璇; 何晓娇

    2011-01-01

    Concentration of atmospheric particles is one of the atmospheric pollution indicators. Heavy metals in the atmospheric particles can risk for human health in both direct and indirect way. Arsenic is one of the higher metal content in them. The inorganic compounds are far more toxic than their organic metabolites. In this paper, the hydride generation atomic fluorescence spectrometric method was employed to the determination of As ( Ⅲ ) and As (V) in the Atmospheric particles. The amount of reducing agent,acid medium and its acidity, carrier gas and shield gas flow rate and observation height of the fluorescence intensity were investigated, and the interference experiment was carried out for concomitant elements. In the best conditions, the detection limit was 0. 34 μg/L, the recovery ranged from 98.18% ~ 102.54%,and the relative standard deviation was about 0.8%. The method was featured by easy operation, fast speed and it has been applied to the analysis of arsenic in the particles with satisfactory results.%采用氢化物发生原子荧光法直接测定不同粒径大气颗粒物中As(Ⅲ)和As(Ⅴ)的含量.研究了还原剂用量、酸介质及其酸度、载气及屏蔽气流量和观测高度等对荧光强度的影响,探讨了共存离子对砷测定的干扰.在选定的最佳条件下,得到检出限为0.34μg/L,方法检出限为0.21μg/g,加标回收率为98.18%~102.54%,相对标准偏差为0.8%左右.用该方法测定大气颗粒物中不同形态的砷,操作简便,快速,灵敏度高.

  9. Non-dispersive atomic-fluorescence spectrometry of trace amounts of bismuth by introduction of its gaseous hydride into a premixed argon (entrained air)-hydrogen flame.

    Science.gov (United States)

    Kobayashi, S; Nakahara, T; Musha, S

    1979-10-01

    A method has been developed for the determination of bismuth by generation of its gaseous hydride and introduction of the hydride into a premixed argon (entrained air)-hydrogen flame, the atomic-fluorescence lines from which are all detected by use of a non-dispersive system. The detection limit is 5 pg/ml, or 0.1 ng of bismuth, but the reagent blank found in a 20-ml sample volume was approximately 2 ng of bismuth. Analytical working curves obtained by measuring peak-heights and integrated peak-areas of the signals are linear over a range of about four orders of magnitude from the detection limit. Perchloric, phosphoric and sulphuric acids up to 2.0M concentration give no interference, but nitric acid gives slight depression of the signal. The presence of silver, gold, nickel, palladium, platinum, selenium and tellurium in 1000-fold ratio to bismuth causes pronounced depression of the signal, whereas mercury and tin slightly enhance the atomic-fluorescence signal. The method has been applied to the determination of bismuth in aluminium-base alloys and sulphide ores with use of the standard additions method. The results are in good agreement with those obtained by flame atomic-absorption spectrometry and optical emission spectrometry with an inductively coupled plasma.

  10. 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

    by electrothermal atomic absorption spectrometry (ETAAS). Based on the dimethylglyoxime (DMG) gravimetric procedure used for nickel analysis, the sample, as contained in pH 9.0 buffer, is, after on-line merging with the chelating reagent, transported to a reaction coil attached to one of the external ports...

  11. Fluorescence spectrometric study of the interaction between inositol and bovine serum albumin%肌醇与牛血清白蛋白相互作用的荧光光谱研究

    Institute of Scientific and Technical Information of China (English)

    王志军; 梁瑞瑞; 雷海英

    2012-01-01

    The interaction between inositol and bovine serum albumin (BSA) at different temperature was investigated by means of fluorescence spectrometry. Quenching constant was obtained, and the effect of inositol on the conformation of BSA was discussed. Moreover, the shortest distance between inositol and BSA was determined based on energy transfer theory. Results show that only dynamic quenching exists between inositol and BSA.%应用荧光光谱研究了肌醇与牛血清白蛋白(BSA)分子间的相互作用;求出了猝灭常数,讨论了肌醇对BSA构象的影响,并依据能量转移理论确定了肌醇与蛋白的最近距离.结果表明,肌醇与BSA两者间的相互作用为单一的动态猝灭过程.

  12. Quantification of ultra-trace amounts of copper by using off-line solid phase extraction-flame atomic absorption spectrometric determination through the octadecyl silica-bonded phase membrane (OSPM) C18 disks impregnated with 2,2'-[ethane-1,2-diylbis(thio)]dianiline.

    Science.gov (United States)

    Mohammadhosseini, Majid; Soliemani, Esmaeil

    2014-07-01

    This study reports a very selective, easy, and precise method for rapid separation of trace amounts of copper in aqueous samples using octadecyl silica-bonded phase membrane disks modified by 2,2'-[ethane-1,2-diylbis(thio)]dianiline (EDTD) combined with flame atomic absorption spectrometric determination. In addition, the synthesis and spectral characterization of EDTD have been described in detail. All the affecting experimental variables such as pH, amount of modifier, eluent type, sample and eluent flow rate, interfering ions, and disk capacity were also investigated. The target analyte (trace copper) was quantitatively retained at pH = 4 and eluted with 6.0 mL of 0.5 M HNO3 at flow rates of 40 and 10 mL min−1 for analyte passage and elution steps, respectively, through the disks modified with 17.0 mg of EDTD. The proposed method also allows an enrichment factor of about 500 and has a detection limit of 0.005 ng mL−1. The method has been successfully applied for isolation and determination of copper in different water samples, peppers, and standard alloys.

  13. 水飞蓟素与牛血清白蛋白相互作用的荧光光谱研究%Fluorescence spectrometric study of interaction between silymarin and bovine serum albumin

    Institute of Scientific and Technical Information of China (English)

    尚永辉; 孙家娟; 刘静

    2011-01-01

    The interaction between silymarin and bovine serum albumin (BSA) in physiological buffer solution (pH = 7.40) as well as the effect of silymarin on the conformation of BSA were studied by means of synchronous fluorescence spectrometry. It was found that silymarin quenched the fluorescence of BSA via a static quenching process, with thermodynamic parameters including enthalpy change (ΔrHm) and entropy change (ΔrSm) being -45. 21 kJ · mol-1 and -61.61 J · K-1· mol-1, respectively. Thus it could be inferred that the interaction between silymarin and BSA was driven mainly by hydrogen bonding and Van der Waals forces, and the binding process was a spontaneous process.%采用同步荧光光谱技术研究了pH=7.40的Tris-HCl缓冲体系中水飞蓟素与牛血清白蛋白(BSA)的相互作用以及水飞蓟素对BSA构象的影响.结果表明,水飞蓟素对BSA的荧光猝灭过程为静态猝灭,结合热力学参数△rH∞=-45.21 kJ·mol-1,△rSm=-61.61 J·K-1·mol-1;据此可以推断,水飞蓟素与BSA之间主要靠氢键和范德华力相结合,其结合过程为自发反应过程.

  14. Measurement of radiative lifetime in atomic samarium using simultaneous detection of laser-induced fluorescence and photoionization signals

    Indian Academy of Sciences (India)

    A C Sahoo; M L Shah; P K Mandal; A K Pulhani; G P Gupta; Vas Dev; B M Suri

    2014-02-01

    In this paper, we report the investigations of lifetime measurement of odd-parity energy level 19009.52 cm-1 of Sm I using simultaneous detection of laser-induced fluorescence and laserinduced photoionization signals employing pump–probe technique. To the best of our knowledge, this is for the first time that the results obtained using laser-induced fluorescence and photoionization techniques have been compared with each other. The obtained results match well with those reported in the literature.

  15. Measurement of K-X-rays fluorescence cross-sections, fluorescence yields and intensity ratios for elements in the atomic range 21 < Z < 74 excited by 59 keV photons

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Avila, J.; Lopez-Pino, N.; Padilla-Cabal, F.; Van Espen, P.; Cabal, A.; Pena, M. Ruiz; Alessandro, K.D.; Maidana, N.L. [Instituto Superior de Tecnologia y Ciencias Aplicadas (InSTEC), La Habana (Cuba); Antwerp Univ. (Belgium). Micro Trace Analytical Center; CEADEN, La Habana (Cuba); Universidade de Sao Paulo (IF/USP), SP (Brazil). Inst. de Fisica. Lab. do Acelerador Linear

    2010-07-01

    Full text: Using 59 keV photons, we measured the K{sub {alpha}}, K{sub {beta}} and total K X-rays fluorescence cross sections of 17 elements in the atomic range 21 < Z < 74. Furthermore, the fluorescence yields and the I{sub K{beta}} / I{sub K{alpha}} intensity ratios for these elements were also determined. An annular radioactive source of {sup 241}Am (activity 1 Ci) was employed to excite the elements in targets with the shape of foils or pellets (99% purity and 20 mm, in diameter). The pellets were formed with a mixture of cellulose and a chemical compound containing the element of interest, pressed at 15 tons. The K X-rays emitted from the irradiated samples were detected by a Si(Li) detector with a frontal Pb collimator, coupled to conventional electronics, with dead time below 10%. The fluxes reaching the targets and the crystal detector were determined by means of Monte Carlo (MC) simulations using the MCNPX V 2.6 code. The input geometries included the detector, the sample-source holder and the Pb collimator. The optimal diameter for the samples as well as the collimator dimensions were estimated by means of MC simulations. Using several elements (Ti, Ni, Br, Ag, Cs, Dy and W) a calibration curve for the effective flux of photons (I{sub 0}G{sub {epsilon}}) as function of the K X-rays energy was measured. Correction by different sizes and self-absorption coefficients of the samples were also performed. The data obtained for the X-rays fluorescence cross sections were compared with semi-empirical calculations and with experimental values reported by other authors; the relative deviations were less than 10%. Keywords: fluorescence cross section, fluorescence yields, Monte Carlo (author)

  16. Single-laboratory validation of a high-performance liquid chromatographic-diode array detector-fluorescence detector/mass spectrometric method for simultaneous determination of water-soluble vitamins in multivitamin dietary tablets.

    Science.gov (United States)

    Chen, Pei; Atkinson, Renata; Wolf, Wayne R

    2009-01-01

    The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors [diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS)] for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phase octadecylsilyl column (4 microm, 250 x 2.0 mm id) and a gradient mobile phase profile. Gradient elution was performed at a flow rate of 0.25 mL/min. After a 5 min isocratic elution at 100% A (0.1% formic acid in water), a linear gradient to 50% A and 50% B (0.1% formic acid in acetonitrile) at 15 min was employed. Detection was performed with a DAD as well as either an FLD or a triple-quadrupole MS detector in the multiple reaction monitoring mode. SLV was performed using Standard Reference Material (SRM) 3280 Multivitamin/Multimineral Tablets, being developed by the National Institute of Standards and Technology, with support by the Office of Dietary Supplements of the National Institutes of Health. Phosphate buffer (10 mM, pH 2.0) extracts of the NIST SRM 3280 were analyzed by the liquid chromatographic (LC)-DAD-FLDIMS method. Following extraction, the method does not require any sample cleanup/preconcentration steps except centrifugation and filtration.

  17. 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

    Science.gov (United States)

    Žemberyová, M.; Jankovič, R.; Hagarová, I.; Kuss, H.-M.

    2007-05-01

    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 HNO 3-HClO 4-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%.

  18. Density relaxation and particle motion characteristics in a non-ionic deep eutectic solvent (acetamide + urea): Time-resolved fluorescence measurements and all-atom molecular dynamics simulations

    Energy Technology Data Exchange (ETDEWEB)

    Das, Anuradha; Das, Suman; Biswas, Ranjit, E-mail: ranjit@bose.res.in [Chemical, Biological and Macromolecular Sciences, S. N. Bose National Centre for Basic Sciences, Block-JD, Sector-III, Salt Lake, Kolkata, West Bengal 700098 (India)

    2015-01-21

    Temperature dependent relaxation dynamics, particle motion characteristics, and heterogeneity aspects of deep eutectic solvents (DESs) made of acetamide (CH{sub 3}CONH{sub 2}) and urea (NH{sub 2}CONH{sub 2}) have been investigated by employing time-resolved fluorescence measurements and all-atom molecular dynamics simulations. Three different compositions (f) for the mixture [fCH{sub 3}CONH{sub 2} + (1 − f)NH{sub 2}CONH{sub 2}] have been studied in a temperature range of 328-353 K which is ∼120-145 K above the measured glass transition temperatures (∼207 K) of these DESs but much lower than the individual melting temperature of either of the constituents. Steady state fluorescence emission measurements using probe solutes with sharply different lifetimes do not indicate any dependence on excitation wavelength in these metastable molten systems. Time-resolved fluorescence anisotropy measurements reveal near-hydrodynamic coupling between medium viscosity and rotation of a dissolved dipolar solute. Stokes shift dynamics have been found to be too fast to be detected by the time-resolution (∼70 ps) employed, suggesting extremely rapid medium polarization relaxation. All-atom simulations reveal Gaussian distribution for particle displacements and van Hove correlations, and significant overlap between non-Gaussian (α{sub 2}) and new non-Gaussian (γ) heterogeneity parameters. In addition, no stretched exponential relaxations have been detected in the simulated wavenumber dependent acetamide dynamic structure factors. All these results are in sharp contrast to earlier observations for ionic deep eutectics with acetamide [Guchhait et al., J. Chem. Phys. 140, 104514 (2014)] and suggest a fundamental difference in interaction and dynamics between ionic and non-ionic deep eutectic solvent systems.

  19. 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.

  20. 电感耦合等离子体光谱法测定童鞋中的铬含量%Inductively Coupled Plasma-Atomic Emission Spectrometric (ICP-AES) Determination of Chromium in Children's Leather Shoes

    Institute of Scientific and Technical Information of China (English)

    刘贵深; 李婷; 侯晓东

    2012-01-01

    采用微波消解-电感耦合等离子体光谱法测定市场上不同厂家生产的童鞋中铬含量,对结果进行分析研究,找出重金属铬超标的原因并提出解决的对策,为降低健康安全风险,提高产品质量提供一定的参考依据。%Chromium content in children's leather shoes from different manufacturer was determined using microwave digestion and inductively coupled plasma-atomic emission spectrometry. This monitoring provides some references to reduce the health and safety risks, and improve the quality of products.

  1. 布朗葡萄藻脂质含量的荧光光谱检测方法的改进%Improved fluorescence spectrometric determination of lipid content in Botryococcus braunii

    Institute of Scientific and Technical Information of China (English)

    刘新颖; 汪志平; 于金鑫; 吕蓓芬; 马丽芳; 陈子元

    2013-01-01

    Botryococcus braunii is a unique colonial green microalga and a great potential renewable resource of liquid fuel because of its ability to produce lipids. Due to the dense cell colonies and rigidly thick cell wall of B. braunii, the traditional Nile red method is usually of low sensitivity and bad repeatability and hard for the determination of lipid content in the cells. By dispersing the colony with ultrasonic, assisting permeation of Nile red across the cell wall with dimethyl sulfoxide and optimizing the staining conditions, we established an improved detection method. The details were as follows: after the colonial algal sample was treated by ultrasonic at 20 kHz for 20 s, 100 W transmitting power and with 1 s on/1 s off intermittent cycle, the equivoluminal 15% (V/V) dimethyl sulfoxide and 3 ng/mL Nile red were successively added and mixed evenly, then the staining system was incubated in dark at 40 ℃ for 10 min, and subsequently was measured by fluorescence spectroscopy detection with an excitation wavelength of 490 nm. Compared with the traditional method, the improved one not only had higher detection sensitivity which was increased by 196.6%, but also had obviously better detection repeatability whose characteristic parameter - relative standard deviation (RSD) was decreased from 10.91% to 1.84%. Therefore, the improved method could provide a rapid and sensitive detection of lipid content for B. braunii breeding and cultivation.%布朗葡萄藻是一种含脂量高、开发潜力大的能源微藻,但因其细胞呈集落态且胞壁较坚厚,应用传统的尼罗红荧光光谱法测定其脂质含量时,通常因灵敏度低、重复性差而难以获得可靠结果.本研究通过超声波分散集落、二甲基亚砜辅助尼罗红进入细胞、优化染色条件,有效地解决了上述问题.具体方法为:藻液先经频率为20 kHz、发射功率为100 W的超声波按1 s/1 s(开/关)间歇处理20 s使细胞分散,而后依

  2. High-resolution multiphoton laser-induced fluorescence spectroscopy of zinc atoms ejected from laser-irradiated ZnS crystals

    Science.gov (United States)

    Arlinghaus, H. F.; Calaway, W. F.; Young, C. E.; Pellin, M. J.; Gruen, D. M.; Chase, L. L.

    1989-01-01

    Time-of-flight (TOF) measurements employing high-resolution multiphoton laser-induced fluorescence spectroscopy (LFS) have been used as a probe to determine the yield and velocity distributions of Zn atoms ejected from a ZnS single crystal under irradiation by 308-nm photons. For fluences between 20 and 80 mJ/cm2 (irradiated area 2 mm2), the velocity distributions could be fitted by Maxwell-Boltzmann distributions where the characteristic temperature increased from 2000 to 9000 K, respectively. The absolute neutral Zn yield also increased from 108 to 1012 atoms per pulse over this same fluence range. Plots of temperature (T) as a function of fluence (F) and yield as a function of 1/T and 1/F suggest thermal evaporation as the mechanism for the Zn emission.The results indicate that with increasing fluence a critical combination of particle density and laser intensity is reached for formation of a plasma which interacts with the surface to cause catastrophic failure. For consecutive laser shots at constant ablation laser fluences, a nearly exponential increase of the Zn particle density was observed, although the measured kinetic temperature remains approximately constant even beyond the onset of visible damage to the ZnS surface. Doppler-shift techniques have been combined with TOF measurements for the first time in order to separate prompt from delayed emission of ablated atoms as well as to probe possible molecular or cluster ejection and fragmentation. Evidence for the latter phenomena was obtained.

  3. Ultra-narrow spectroscopic cells in atomic spectroscopy: reflection, transmission, fluorescence, and nonadiabatic transitions at the walls

    Science.gov (United States)

    Pazgalev, A.; Sarkisyan, D.; Cartaleva, S.; Przhibelskii, S.; Vartanyan, T.

    2014-11-01

    Ultra-narrow cells with the thicknesses in the range from several wavelengths to the small fractions of the wavelength brought a number of new opportunities for atomic spectroscopy. Depending on the cell thickness, spectral lines recorded in ultra-narrow cells are either Doppler-free or Doppler-broadened. With careful selection of the cell thickness hyperfine structure may be easily resolved without resorting on the multibeam nonlinear optical techniques. Moreover, frequent collisions with the walls leads to the important modifications of velocity selective optical pumping resonances. Finally, ultra-narrow cells provide with the unique opportunity to study collisions of the excited atoms with the solid surfaces. In this contribution several examples of the use of the ultra-narrow spectroscopic cells filled with the alkali atomic vapour is presented. First, we discuss general aspects of the transient polarisation that defines all peculiarities of an ultra-narrow cell as a spectroscopic tool. Second, we demonstrate the resolution of the magnetic sublevels in the transition from Zeeman to Paschen-Back regime in the Cs hyperfine structure. Third, new aspects of velocity selective optical pumping resonances in reflection and transmission of resonant radiation by the 6 wavelengths thick cell filled with Cs are discussed. Forth, the experimental evidences of the nonadiabatic transitions between excited states of Rb atoms in the course of collisions with the sapphire surface are presented.

  4. Surface passivation of nano-textured fluorescent SiC by atomic layer deposited TiO2

    DEFF Research Database (Denmark)

    Lu, Weifang; Ou, Yiyu; Jokubavicius, Valdas;

    2016-01-01

    Nano-textured surfaces have played a key role in optoelectronic materials to enhance the light extraction efficiency. In this work, morphology and optical properties of nano-textured SiC covered with atomic layer deposited (ALD) TiO2 were investigated. In order to obtain a high quality surface fo...

  5. Cloud point extraction of copper, lead, cadmium, and iron using 2,6-diamino-4-phenyl-1,3,5-triazine and nonionic surfactant, and their flame atomic absorption spectrometric determination in water and canned food samples.

    Science.gov (United States)

    Citak, Demirhan; Tuzen, Mustafa

    2012-01-01

    A cloud point extraction procedure was optimized for the separation and preconcentration of lead(II), cadmium(II), copper(II), and iron(III) ions in various water and canned food samples. The metal ions formed complexes with 2,6-diamino-4-phenyl-1,3,5-triazine that were extracted by surfactant-rich phases in the nonionic surfactant Triton X-114. The surfactant-rich phase was diluted with 1 M HNO3 in methanol prior to its analysis by flame atomic absorption spectrometry. The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, surfactant concentration, temperature, and incubation time, were optimized. LOD values based on three times the SD of the blank (3Sb) were 0.38, 0.48, 1.33, and 1.85 microg/L for cadmium(II), copper(II), lead(II), and iron(III) ions, respectively. The precision (RSD) of the method was in the 1.86-3.06% range (n=7). Validation of the procedure was carried out by analysis of National Institute of Standards and Technology Standard Reference Material (NIST-SRM) 1568a Rice Flour and GBW 07605 Tea. The method was applied to water and canned food samples for determination of metal ions.

  6. Preconcentration of Pb(II), Cr(III), Cu(II), Ni(II) and Cd(II) ions in environmental samples by membrane filtration prior to their flame atomic absorption spectrometric determinations

    Energy Technology Data Exchange (ETDEWEB)

    Divrikli, Umit [Pamukkale University, Faculty of Arts and Science, Department of Chemistry, 20020 Denizli (Turkey)]. E-mail: udivrikli@pamukkale.edu.tr; Kartal, Aslihan Arslan [Pamukkale University, Faculty of Arts and Science, Department of Chemistry, 20020 Denizli (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Arts and Science, Department of Chemistry, 38039 Kayseri (Turkey); Elci, Latif [Pamukkale University, Faculty of Arts and Science, Department of Chemistry, 20020 Denizli (Turkey)

    2007-07-16

    A method for separation-preconcentration of Pb(II), Cr(III), Cu(II), Ni(II) and Cd(II) ions by membrane filtration has been described. The method based on the collection of analyte metal ions on a cellulose nitrate membrane filter and determination of analytes by flame atomic absorption spectrometry (FAAS). The method was optimized for several parameters including of pH, matrix effects and sample volume. The recoveries of analytes were generally in the range of 93-100%. The detection limits by 3 sigma for analyte ions were 0.02 {mu}g L{sup -1} for Pb(II), 0.3 {mu}g L{sup -1} for Cr(III), 3.1 {mu}g L{sup -1} for Cu(II), 7.8 {mu}g L{sup -1} for Ni(II) and 0.9 {mu}g L{sup -1} for Cd(II). The proposed method was applied to the determination of lead, chromium, copper, nickel and cadmium in tap waters and RM 8704 Buffalo River Sediment standard reference material with satisfactory results. The relative standard deviations of the determinations were below 10%.

  7. Study on the Inclusion Interactions of Cucurbit[7]uril with 6-Mercaptopurine and Adenine by Fluorescence Spectrometric Method%荧光光谱法研究葫芦[7]脲与6-巯嘌呤和腺嘌呤的包结作用

    Institute of Scientific and Technical Information of China (English)

    何小英; 李来生; 方奕珊; 陈红

    2012-01-01

    The inclusion interactions of cucurbit [7] uril (CB[7]) with 6-mercaptopurine (6-MP) and adenine(ADP) were studied by fluorescence spectrometric method. Several effect factors such as time, the pH value and temperature on the fluorescence intensity and the stability of the complex were investigated. The complex constants of CB[7] with 6-MP and ADP were determined according to the Benesi-Hildebrand equation,respectively. The results indicated that the pH value had a significant effect on the inclusion interactions. 6-MP and ADP had the optimal and stable excitation and emission wavelength as the pH value were 8. 0 for 6-MP and 2. 0 for ADP within 5 min. With the increasing of the concentrations of CB[7],the fluorescence of the two complexes increased obviously. The inclusion constants were 3. 6797× 102 L·mol-1 for 6-MP-CB[7] and 2. 2033 × 102 L·mol-1 for ADP-CB[7] at 298 K with the same inclusive ratio of It 1. The main interaction forces between CB[7] and the above purines were discussed based on the thermodynamic parameters. CB[7] is only well water-soluble superamolecules among cucurbituril family members, and has great potential as drug carriers with safety and low toxicity.%采用荧光光谱法分别研究了葫芦[7]脲(CB[7])对6-巯嘌呤(6-MP)和腺嘌呤(ADP)的包结作用.实验考察了时间、pH值以及温度对荧光强度和包结作用的影响,利用Benesi-Hildebrand方程分别计算出6-MP和ADP与CB[7]的包结常数.结果表明:酸度对体系的包结有明显的影响.在pH值为8.0和2.0左右时,6-MP和ADP分别具有稳定和最佳激发和发射波长,随着CB[7]浓度的增大,体系的荧光强度都有明显增强,包结作用迅速(小于5 min).实验得出CB[7]与6-MP和ADP的包结比均为1∶1,在298 K时的包结常数分别为3.6797×102 L·mol-1和2.2033×102 L·mo1-1.通过热力学参数的变化,探讨了维系包结物稳定性的主要作用力.CB[7]是葫芦脲家族中水溶性最强的主体分子,作为一种

  8. Comparison of nanosecond and picosecond excitation for interference-free two-photon laser-induced fluorescence detection of atomic hydrogen in flames.

    Science.gov (United States)

    Kulatilaka, Waruna D; Patterson, Brian D; Frank, Jonathan H; Settersten, Thomas B

    2008-09-10

    Two-photon laser-induced fluorescence (TP-LIF) line imaging of atomic hydrogen was investigated in a series of premixed CH4/O2/N2, H2/O2, and H2/O2/N2 flames using excitation with either picosecond or nanosecond pulsed lasers operating at 205 nm. Radial TP-LIF profiles were measured for a range of pulse fluences to determine the maximum interference-free signal levels and the corresponding picosecond and nanosecond laser fluences in each of 12 flames. For an interference-free measurement, the shape of the TP-LIF profile is independent of laser fluence. For larger fluences, distortions in the profile are attributed to photodissociation of H2O, CH3, and/or other combustion intermediates, and stimulated emission. In comparison with the nanosecond laser, excitation with the picosecond laser can effectively reduce the photolytic interference and produces approximately an order of magnitude larger interference-free signal in CH4/O2/N2 flames with equivalence ratios in the range of 0.5laser fluence in all flames, stimulated emission, occurring between the laser-excited level, H(n=3), and H(n=2), is the limiting factor for picosecond excitation in the flames with the highest H atom concentration. Nanosecond excitation is advantageous in the richest (Phi=1.64) CH4/O2/N2 flame and in H2/O2/N2 flames. The optimal excitation pulse width for interference-free H atom detection depends on the relative concentrations of hydrogen atoms and photolytic precursors, the flame temperature, and the laser path length within the flame.

  9. Bovine serum albumin-Cu(II) hybrid nanoflowers: An effective adsorbent for solid phase extraction and slurry sampling flame atomic absorption spectrometric analysis of cadmium and lead in water, hair, food and cigarette samples

    Energy Technology Data Exchange (ETDEWEB)

    Yilmaz, Erkan [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey); Ocsoy, Ismail [Department of Analytical Chemistry, Faculty of Pharmacy, Erciyes University, Kayseri 38039 (Turkey); Nanotechnology Research Center (ERNAM), Erciyes University, Kayseri 38039 (Turkey); Ozdemir, Nalan [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey); Soylak, Mustafa, E-mail: soylak@erciyes.edu.tr [Department of Chemistry, Faculty of Sciences, Erciyes University, Kayseri 38039 (Turkey)

    2016-02-04

    Herein, the synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers (BSA-NFs) through the building blocks of bovine serum albumin (BSA) and copper(II) ions in phosphate buffered saline (PBS) and their use as adsorbent for cadmium and lead ions are reported. The BSA-NFs, for the first time, were efficiently utilized as novel adsorbent for solid phase extraction (SPE) of cadmium and lead ions in water, food, cigarette and hair samples. The method is based on the separation and pre-concentration of Cd(II) and Pb(II) by BSA-NFs prior to determination by slurry analysis via flame atomic absorption spectrometry (FAAS). The analytes were adsorbed on BSA-NFs under the vortex mixing and then the ion-loaded slurry was separated and directly introduced into the flame AAS nebulizer by using a hand-made micro sample introduction system to eliminate a number of drawbacks. The effects of analytical key parameters, such as pH, amount of BSA-NFs, vortexing time, sample volume, and matrix effect of foreign ions on adsorbing of Cd(II) and Pb(II) were systematically investigated and optimized. The limits of detection (LODs) for Cd(II) and Pb(II) were calculated as 0.37 μg L{sup −1} and 8.8 μg L{sup −1}, respectively. The relative standard deviation percentages (RSDs) (N = 5) for Cd(II) and Pb(II) were 7.2%, and 5.0%, respectively. The accuracy of the developed procedure was validated by the analysis of certified reference materials (TMDA-53.3 Fortified Water, TMDA-70 Fortified Water, SPS-WW2 Waste Water, NCSDC-73349 Bush Branches and Leaves) and by addition/recovery analysis. The quantitative recoveries were obtained for the analysis of certified reference materials and addition/recovery tests. The method was successfully applied to the analysis of cadmium and lead in water, food, cigarette and hair samples. - Highlights: • The synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers is reported. • The nanoflowers were utilized for solid phase microextraction of

  10. 人血和尿中锡的高压微波络合消解氢化物发生-原子荧光测定法%Determination of tin in human blood and urine with high-pressure microwave digestion and complexing ligand and hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    陈峰; 谢超

    2013-01-01

    Objective To establish the hydride generation-atomic fluorescence spectrometric method for the determination of tin in human blood and urine with high-pressure microwave digestion and complexing ligand.Methods Human blood and urine samples were digested by using high-pressure microwave.Then complexing ligand 1% EDTA,5 ml 150 g/L thiourea and ascorbic acid were added to mask the interfering ions such as nickel,iron,arsenic,selenium and etc.Tin concentration was determined with hydride-generation atomic fluorescence spectrometric method with sodium borohydride as the reductant in 2% sulphuric acid media.Results The linear range of tin was 10-100 μg/ml,the regression equations and correlation coefficients in blood and urine were y=9.391 1 x-16.312,r=0.999 7,y=8.244 7x-27.849 6,r=0.998 2,respectively.The limits of detection of tin in blood and urine were 0.090,0.020 μg/L respectively.The relative standard derivation of this method was 1.4%-6.1%.The rates of recovery were between 98.1% and 101.8%.Conclusion This method presents many advantages,such as completed sample digestion,rapid,less matrix disturbance,accurate,sensitive and is applicable to the determination of tin in blood and urine in grass-roots units.%目的 建立人血、尿中锡的高压微波络合消解氢化物发生-原子荧光测定法.方法 利用高压微波络合消解已加入1% EDTA溶液的人血和尿液,在样品测定液中加入150 g/L硫脲-抗坏血酸5ml来掩蔽镍、铁、砷、硒等干扰离子;以2%硫酸作为介质,以2%的硼氢化钠溶液作为还原剂,采用氢化物发生-原子荧光法测定锡浓度.结果 在10~100 μg/ml的线性范围内,血中锡所得回归方程为y=9.391 1x-16.312,r=0.999 7;尿中锡所得回归方程为y=8.244 7x-27.849 6,r=0.998 2.血、尿中锡的检出限分别为0.090、0.020 μg/L.该方法的RSD为1.4%~6.1%,回收率在98.1%~101.8%之间.结论 该方法样品消解完全,测定时间短,待测元素

  11. Diagnostics of Carbon Nanotube Formation in a Laser Produced Plume: An Investigation of the Metal Catalyst by Laser Ablation Atomic Fluorescence Spectroscopy

    Science.gov (United States)

    deBoer, Gary; Scott, Carl

    2003-01-01

    Carbon nanotubes, elongated molecular tubes with diameters of nanometers and lengths in microns, hold great promise for material science. Hopes for super strong light-weight material to be used in spacecraft design is the driving force behind nanotube work at JSC. The molecular nature of these materials requires the appropriate tools for investigation of their structure, properties, and formation. The mechanism of nanotube formation is of particular interest because it may hold keys to controlling the formation of different types of nanotubes and allow them to be produced in much greater quantities at less cost than is currently available. This summer's work involved the interpretation of data taken last summer and analyzed over the academic year. The work involved diagnostic studies of carbon nanotube formation processes occurring in a laser-produced plume. Laser ablation of metal doped graphite to produce a plasma plume in which carbon nanotubes self assemble is one method of making carbon nanotube. The laser ablation method is amenable to applying the techniques of laser spectroscopy, a powerful tool for probing the energies and dynamics of atomic and molecular species. The experimental work performed last summer involved probing one of the metal catalysts, nickel, by laser induced fluorescence. The nickel atom was studied as a function of oven temperature, probe laser wavelength, time after ablation, and position in the laser produced plume. This data along with previously obtained data on carbon was analyzed over the academic year. Interpretations of the data were developed this summer along with discussions of future work. The temperature of the oven in which the target is ablated greatly influences the amount of material ablated and the propagation of the plume. The ablation conditions and the time scale of atomic and molecular lifetimes suggest that initial ablation of the metal doped carbon target results in atomic and small molecular species. The metal

  12. 检定原子荧光光度计常见问题分析%Atomic Fluorescence Spectrophotometer Calibration Common Problems

    Institute of Scientific and Technical Information of China (English)

    童诚; 吴银银; 马文

    2015-01-01

    This paper presents the common problems of possible atomic fluorescence spectrophotometer verification process .According to the working principle of the instrument and the experience , causes of the problems were analyzed , and specific solutions were proposed for different problems.It can guarantee accurate and reliable verification results .%提出了原子荧光光度计检定过程中可能出现的常见问题。根据经验和仪器的工作原理对问题产生的原因进行了分析,并针对不同问题给出了具体的解决措施。对实现检定结果的准确可靠具有较好的保证作用。

  13. Intracellular concentration map of magnesium in whole cells by combined use of X-ray fluorescence microscopy and atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Lagomarsino, Stefano, E-mail: stefano.lagomarsino@cnr.it [IPCF-CNR -UOS Roma c/o Dip Fisica Universita' ' Sapienza' , P.le A. Moro, 2 Rome (Italy); Physics Department, Universita' Sapienza, P.le A. Moro, 2 Rome (Italy); Iotti, Stefano [Dipartimento di Medicina Interna, dell' Invecchiamento e Malattie Nefrologiche Universita di Bologna, Via Massarenti, 9 40138 Bologna (Italy); Istituto Nazionale Biostrutture e Biosistemi - Rome (Italy); Farruggia, Giovanna [Dipartimento di Biochimica ' G. Moruzzi' Universita di Bologna, Via Irnerio, 48 40126 Bologna (Italy); Cedola, Alessia [IFN-CNR - V. Cineto Romano, 42 00156 Rome (Italy); Trapani, Valentina [Istituto di Patologia Generale - Universita Cattolica del Sacro Cuore - Facolta di Medicina ' A. Gemelli' L.go F. Vito, 1 00168 Rome (Italy); Fratini, Michela [IFN-CNR - V. Cineto Romano, 42 00156 Rome (Italy); Bukreeva, Inna [IFN-CNR - V. Cineto Romano, 42 00156 Rome (Italy); Shubnikov Institute of Crystallography, Leninskii prospekt 59, Moscow, 119333 (Russian Federation); Notargiacomo, Andrea [IFN-CNR - V. Cineto Romano, 42 00156 Rome (Italy); Mastrototaro, Lucia [Istituto di Patologia Generale - Universita Cattolica del Sacro Cuore - Facolta di Medicina ' A. Gemelli' L.go F. Vito, 1 00168 Rome (Italy); Marraccini, Chiara [Dipartimento di Medicina Interna, dell' Invecchiamento e Malattie Nefrologiche Universita di Bologna, Via Massarenti, 9 40138 Bologna (Italy); and others

    2011-11-15

    We report a novel experimental approach to derive quantitative concentration map of light elements in whole cells by combining two complementary nano-probe methods: X-ray fluorescence microscopy (XRFM) and atomic force microscopy (AFM). The concentration is derived by normalizing point-by-point the elemental (here Mg) spatial distribution obtained by XRFM, by the thickness measured using AFM. The considerable difference between the elemental distribution and the concentration maps indicates that this procedure is essential to obtain reliable information on the role and function of elements in whole cells. - Highlights: Black-Right-Pointing-Pointer X-ray fluorescence and AFM have been measured on the same de-hydrated whole cells. Black-Right-Pointing-Pointer The element distribution has been normalized point-by-point by the cell thickness. Black-Right-Pointing-Pointer The element (Mg) concentration map has been obtained on a whole cell. Black-Right-Pointing-Pointer The element concentration map is quite different from the distribution map. Black-Right-Pointing-Pointer Higher Mg concentration is found in the cell periphery.

  14. 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.

  15. Speciation analysis by gas chromatography with plasma source spectrometric detection

    Science.gov (United States)

    Łobiński, Ryszard; Adams, Freddy C.

    State-of-the-art species-selective analysis by gas chromatography (GC) with plasma source spectrometric detection is discussed for organometal and organometalloid compounds. Various plasmas, inductively coupled plasma, microwave induced plasma, capacitatively coupled plasma, direct current plasma and alternating current plasma, are characterized and critically compared as sources of radiation for atomic emission spectrometry and sources of ions for mass spectrometry. Interfaces between gas chromatography (packed, wide-bore, capillary and multicapillary) and plasma source spectrometry are characterized. Particular emphasis is given to applications of GC with plasma source detection to real-world analytical problems, which are comprehensively reviewed. The use of plasmas for the acquisition of auxiliary molecular information such as empirical formulae and structural information is discussed. Recent developments relating to sample preparation and presentation to the hyphenated system are addressed. The most significant trends in speciation analysis are highlighted.

  16. Spatial dynamics of laser-induced fluorescence in an intense laser beam: experiment and theory in alkali metal atoms

    CERN Document Server

    Auzinsh, Marcis; Ferber, Ruvin; Gahbauer, Florian; Kalnins, Uldis

    2015-01-01

    We have shown that it is possible to model accurately optical phenomena in intense laser fields by taking into account the intensity distribution over the laser beam. We developed a theoretical model that divided an intense laser beam into concentric regions, each with a Rabi frequency that corresponds to the intensity in that region, and solved a set of coupled optical Bloch equations for the density matrix in each region. Experimentally obtained magneto-optical resonance curves for the $F_g=2\\longrightarrow F_e=1$ transition of the $D_1$ line of $^{87}$Rb agreed very well with the theoretical model up to a laser intensity of around 200 mW/cm$^2$ for a transition whose saturation intensity is around 4.5 mW/cm$^2$. We have studied the spatial dependence of the fluorescence intensity in an intense laser beam experimentally and theoretically. An experiment was conducted whereby a broad, intense pump laser excited the $F_g=4\\longrightarrow F_e=3$ transition of the $D_2$ line of cesium while a weak, narrow probe ...

  17. Determination of monomethylmercury in low- and high-polluted sediments by microwave extraction and gas chromatography with atomic fluorescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Berzas Nevado, J.J. [Regional Institute for Applied Scientific Research, University of Castilla-La Mancha, E-13071 Ciudad Real (Spain); Rodriguez Martin-Doimeadios, R.C. [Department of Analytical Chemistry and Food Technology, Faculty of Environmental Sciences, University of Castilla-La Mancha, Avda. Carlos III s/n, E-45071 Toledo (Spain)], E-mail: RosaCarmen.Rodriguez@uclm.es; Guzman Bernardo, F.J.; Jimenez Moreno, M. [Department of Analytical Chemistry and Food Technology, Faculty of Environmental Sciences, University of Castilla-La Mancha, Avda. Carlos III s/n, E-45071 Toledo (Spain)

    2008-02-04

    The analysis of monomethylmercury (MMHg) in sediments is a difficult task because both very low concentrations and interconversion between species especially in highly polluted samples are frequent. This work features a general strategy for real sediment analysis with preconcentration and/or clean-up steps for both low- and high-polluted sediments to control these specific problems. The extraction conditions have been optimized using closed-vessel microwave-assisted heating with acidic extractants. The analysis has been carried out by the injection of ethylated derivatives of the analytes into a capillary gas chromatographic system coupled to fluorescence spectrometry. When using 6 M HNO{sub 3}, the most labile inorganic mercury fraction as well as MMHg were extracted from the sediment but there was still some inorganic mercury that remained un-extracted. MMHg was stable and quantitatively recovered by applying this procedure. The role of the labile inorganic fraction on artifact MMHg generation has been evaluated and it has been found to be highly variable depending on the sediments' geochemical characteristics. Therefore, for high-polluted sediments (inorganic mercury concentration above 500 ng g{sup -1}) a clean-up step with dichloromethane has been used before ethylation, whereas for low content samples, preconcentration under nitrogen stream at room temperature has been optimized. Both steps can be combined if necessary. MMHg content has been found in good agreement with the certified value for the reference materials (IAEA-405 and ERM-CC580)

  18. [Cloud Point extraction for determination of mercury in Chinese herbal medicine by hydride generation atomic fluorescence spectrometry with optimization using Box-Behnken design].

    Science.gov (United States)

    Wang, Mei; Li, Shan; Zhou, Jian-dong; Xu, Ying; Long, Jun-biao; Yang, Bing-yi

    2014-08-01

    Cloud point extraction (CPE) is proposed as a pre-concentration procedure for the determination of Hg in Chinese herbal medicine samples by hydride generation-atomic fluorescence spectrometry (HG-AFS). Hg2+ was reacted with dithizone to form hydrophobic chelate under the condition of pH. Using Triton X-114, as surfactant, chelate was quantitatively extracted into small volume of the surfactant-rich phase by heating the solution in a water bath for 15 min and centrifuging. Four variables including pH, dithizone concentration, Triton X-114 concentration and equilibrium temperature (T) showed the significant effect on extraction efficiency of total Hg evaluated by single-factor experiment, and Box-Behnken design and response surface method- ology were adopted to further investigate the mutual interactions between these variables and to identify their optimal values that would generate maximum extraction efficiency. The results showed that the binomial was used to fit the response to experimental levels of each variable. ALL linear, quadratic terms of four variables, and interactions between pH and Trion X-114, pH and di- thizone affected the response value(extraction efficiency) significantly at 5% level. The optimum extraction conditions were as follows: pH 5.1, Triton X-114 concentration of 1.16 g x L(-1), dithizone concentration of 4.87 mol x L(-1), and T 58.2 degrees C, the predicted value of fluorescence was 4528.74 under the optimum conditions, and the experimental value had only 2.1% difference with it. Under the conditions, fluorescence was linear to mercury concentration in the range of 1-5 microg x L(-1). The limit of detection obtained was 0.01247 microg x L(-1) with the relative standard deviations (R.S.D.) for six replicate determinations of 1.30%. The proposed method was successfully applied to determination of Hg in morindae Radix, Andrographitis and dried tangerine samples with the recoveries of 95.0%-100.0%. Apparently Box-Behnken design combined with

  19. Arsenic speciation in edible alga samples by microwave-assisted extraction and high performance liquid chromatography coupled to atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Salgado, S. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Quijano, M.A., E-mail: marian.quijano@upm.es [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain); Bonilla, M.M. [Departamento de Ingenieria Civil: Tecnologia Hidraulica y Energetica, Escuela Universitaria de Ingenieria Tecnica de Obras Publicas, Universidad Politecnica de Madrid, Alfonso XII 3 y 5, 28014 Madrid (Spain)

    2012-02-10

    Highlights: Black-Right-Pointing-Pointer Total As and As species were analyzed in edible marine algae. Black-Right-Pointing-Pointer A microwave-assisted extraction method with deionized water was applied. Black-Right-Pointing-Pointer As compounds identified comprised DMA, As(V) and four arsenosugars Black-Right-Pointing-Pointer Considerably high As(V) concentrations were found in the most of the algae studied. - Abstract: Twelve commercially available edible marine algae from France, Japan and Spain and the certified reference material (CRM) NIES No. 9 Sargassum fulvellum were analyzed for total arsenic and arsenic species. Total arsenic concentrations were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after microwave digestion and ranged from 23 to 126 {mu}g g{sup -1}. Arsenic species in alga samples were extracted with deionized water by microwave-assisted extraction and showed extraction efficiencies from 49 to 98%, in terms of total arsenic. The presence of eleven arsenic species was studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation atomic-fluorescence spectrometry (HPLC-(UV)-HG-AFS) developed methods, using both anion and cation exchange chromatography. Glycerol and phosphate sugars were found in all alga samples analyzed, at concentrations between 0.11 and 22 {mu}g g{sup -1}, whereas sulfonate and sulfate sugars were only detected in three of them (0.6-7.2 {mu}g g{sup -1}). Regarding arsenic toxic species, low concentration levels of dimethylarsinic acid (DMA) (<0.9 {mu}g g{sup -1}) and generally high arsenate (As(V)) concentrations (up to 77 {mu}g g{sup -1}) were found in most of the algae studied. The results obtained are of interest to highlight the need to perform speciation analysis and to introduce appropriate legislation to limit toxic arsenic species content in these food products.

  20. Femtosecond, two-photon-absorption, laser-induced-fluorescence (fs-TALIF) imaging of atomic hydrogen and oxygen in non-equilibrium plasmas

    Science.gov (United States)

    Schmidt, Jacob B.; Roy, Sukesh; Kulatilaka, Waruna D.; Shkurenkov, Ivan; Adamovich, Igor V.; Lempert, Walter R.; Gord, James R.

    2017-01-01

    Femtosecond, two-photon-absorption laser-induced fluorescence (fs-TALIF) is employed to measure space- and time-resolved distributions of atomic hydrogen and oxygen in moderate-pressure, non-equilibrium, nanosecond-duration pulsed-discharge plasmas. Temporally and spatially resolved hydrogen and oxygen TALIF images are obtained over a range of low-temperature plasmas in mixtures of helium and argon at 100 Torr total pressure. The high-peak-intensity, low-average-energy fs pulses combined with the increased spectral bandwidth compared to traditional ns-duration laser pulses provide a large number of photon pairs that are responsible for the two-photon excitation, which results in an enhanced TALIF signal. Krypton and xenon TALIF are used for quantitative calibration of the hydrogen and oxygen concentrations, respectively, with similar excitation schemes being employed. This enables 2D collection of atomic-hydrogen and -oxygen TALIF signals with absolute number densities ranging from 2  ×  1012 cm-3 to 6  ×  1015 cm-3 and 1  ×  1013 cm-3 to 3  ×  1016 cm-3, respectively. These 2D images are the first application of TALIF imaging in moderate-pressure plasma discharges. 1D self-consistent modeling predictions show agreement with experimental results within the estimated experimental error of 25%. The present results can be used to further the development of higher fidelity kinetic models while quantifying plasma-source characteristics.

  1. Automated dispersive liquid-liquid microextraction coupled to high performance liquid chromatography - cold vapour atomic fluorescence spectroscopy for the determination of mercury species in natural water samples.

    Science.gov (United States)

    Liu, Yao-Min; Zhang, Feng-Ping; Jiao, Bao-Yu; Rao, Jin-Yu; Leng, Geng

    2017-04-14

    An automated, home-constructed, and low cost dispersive liquid-liquid microextraction (DLLME) device that directly coupled to a high performance liquid chromatography (HPLC) - cold vapour atomic fluorescence spectroscopy (CVAFS) system was designed and developed for the determination of trace concentrations of methylmercury (MeHg(+)), ethylmercury (EtHg(+)) and inorganic mercury (Hg(2+)) in natural waters. With a simple, miniaturized and efficient automated DLLME system, nanogram amounts of these mercury species were extracted from natural water samples and injected into a hyphenated HPLC-CVAFS for quantification. The complete analytical procedure, including chelation, extraction, phase separation, collection and injection of the extracts, as well as HPLC-CVAFS quantification, was automated. Key parameters, such as the type and volume of the chelation, extraction and dispersive solvent, aspiration speed, sample pH, salt effect and matrix effect, were thoroughly investigated. Under the optimum conditions, linear range was 10-1200ngL(-1) for EtHg(+) and 5-450ngL(-1) for MeHg(+) and Hg(2+). Limits of detection were 3.0ngL(-1) for EtHg(+) and 1.5ngL(-1) for MeHg(+) and Hg(2+). Reproducibility and recoveries were assessed by spiking three natural water samples with different Hg concentrations, giving recoveries from 88.4-96.1%, and relative standard deviations <5.1%.

  2. An evaluation of the bioaccessibility of arsenic in corn and rice samples based on cloud point extraction and hydride generation coupled to atomic fluorescence spectrometry.

    Science.gov (United States)

    Castor, José Martín Rosas; Portugal, Lindomar; Ferrer, Laura; Hinojosa-Reyes, Laura; Guzmán-Mar, Jorge Luis; Hernández-Ramírez, Aracely; Cerdà, Víctor

    2016-08-01

    A simple, inexpensive and rapid method was proposed for the determination of bioaccessible arsenic in corn and rice samples using an in vitro bioaccessibility assay. The method was based on the preconcentration of arsenic by cloud point extraction (CPE) using o,o-diethyldithiophosphate (DDTP) complex, which was generated from an in vitro extract using polyethylene glycol tert-octylphenyl ether (Triton X-114) as a surfactant prior to its detection by atomic fluorescence spectrometry with a hydride generation system (HG-AFS). The CPE method was optimized by a multivariate approach (two-level full factorial and Doehlert designs). A photo-oxidation step of the organic species prior to HG-AFS detection was included for the accurate quantification of the total As. The limit of detection was 1.34μgkg(-1) and 1.90μgkg(-1) for rice and corn samples, respectively. The accuracy of the method was confirmed by analyzing certified reference material ERM BC-211 (rice powder). The corn and rice samples that were analyzed showed a high bioaccessible arsenic content (72-88% and 54-96%, respectively), indicating a potential human health risk.

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

    Science.gov (United States)

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

    2015-03-01

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

  4. Studies in hydride generation atomic fluorescence determination of selenium and tellurium. Part 1 — self interference effect in hydrogen telluride generation and the effect of KI

    Science.gov (United States)

    D'Ulivo, A.; Marcucci, K.; Bramanti, E.; Lampugnani, L.; Zamboni, R.

    2000-08-01

    The effects of tetrahydroborate (0.02-1%) and iodide (0-3 M) were investigated in determination of tellurium and selenium by hydride generation atomic fluorescence spectrometry. The effect of tetrahydroborate and iodide concentration were tested on the shape of calibration curves in concentration range of 1-1000 ng ml -1 analyte. Reductant deficiency resulted in a moderate sensitivity depression for tellurium but dramatically reduced the useful dynamic range down to 50 ng ml -1. On the contrary, selenium calibration curves retained a linear character even under conditions generating strong sensitivity depression. Curvature and rollover of tellurium calibration curves has been addressed to a self-interference effect caused by the formation of finely dispersed elemental tellurium. Iodide ions were found to have beneficial or no negative effects in the hydrogen telluride generation. Addition of iodide on-line to the sample has been proved effective in the control of the self-interference effect and allows to work in mild reaction conditions. Moreover, it allows a good control of Cu(II) interference and eliminates Ni(II) and Co(II) interferences. The method has been successfully applied to determination of tellurium in copper and lead ores certified reference materials.

  5. 原子荧光光谱法测定环境空气中锑%Antimony Determination by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    顾志勇

    2014-01-01

    采用过氯乙烯滤膜采集环境空气中锑,盐酸-氢氟酸混酸体系微波消解滤膜,原子荧光光谱法测定锑。方法前处理操作过程简单、省时、酸用量少、环境污染小,方法的灵敏度和准确度都有很大的提高。采样体积为300L时,空气中锑的最低检出质量浓度为0.002mg/m3。%Antimony in air was sampled using perchloroethylene filter.The filter was dipped into hydrochloric acid and hydrofluoric acid system and digested by microwave.Atomic fluorescence spectrometry was used to detect anti-mony after.This process is simple and time-saving with easy pretreatment,less amount of acid,and less negative impacts on environment.In addition,the accuracy and precision of the process is better than previous methods. The detection limit of antimony in air is 0.002mg/m3 when the volume of air sample is 300 liters when this process was applied.

  6. Solid Phase Extraction of Inorganic Mercury Using 5-Phenylazo-8-hydroxyquinoline and Determination by Cold Vapor Atomic Fluorescence Spectroscopy in Natural Water Samples

    Science.gov (United States)

    Daye, Mirna; Halwani, Jalal; Hamzeh, Mariam

    2013-01-01

    8-Hydroxyquinoline (8-HQ) was chosen as a powerful ligand for Hg solid phase extraction. Among several chelating resins based on 8-HQ, 5-phenylazo-8-hydroxyquinoline (5Ph8HQ) is used for mercury extraction in which the adsorption dynamics were fully studied. It has been shown that Hg(II) is totally absorbed by 5Ph8HQ within the first 30 minutes of contact time with t1/2 5 minutes, following Langmuir adsorption model. At pH 4, the affinity of mercury is unchallenged by other metals except, for Cu(II), which have shown higher Kd value. With these latter characteristics, 5Ph8HQ was examined for the preconcentration of trace levels of Hg(II). The developed method showed quantitative recoveries of Hg(II) with LOD = 0.21 pg mL−1 and RSD = 3–6% using cold vapor atomic fluorescence spectroscopy (CV-AFS) with a preconcentration factor greater than 250. PMID:24459417

  7. Organic solvent-free reversed-phase ion-pairing liquid chromatography coupled to atomic fluorescence spectrometry for organoarsenic species determination in several matrices.

    Science.gov (United States)

    Monasterio, Romina P; Londonio, Juan A; Farias, Silvia S; Smichowski, Patricia; Wuilloud, Rodolfo G

    2011-04-27

    A novel method has been developed to determine As-containing animal feed additives including roxarsone (ROX), p-arsanilic acid (p-ASA) and nitarsone (NIT), as well as other organic As species (dimethylarsonic acid (DMAA) and monomethylarsonic acid (MMAA)) by ion-pairing high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry (IP-HPLC-HG-AFS). A simple isocratic reversed-phase (RP) HPLC method with a mobile phase containing citric acid and sodium hexanesulfonate (pH 2.0) was developed using a C(18) column. The use of an organic solvent free mobile phase turns this methodology into an environmentally friendly alternative. Several ion pair forming agents, such as sodium hexanesulfonate, tetrabutylammonium bisulfate and perfluoroheptanoic acid, were studied. The limits of detection for As species were calculated in standard solution and resulted to be 0.2, 0.5, 0.6, 1.6, and 1.6 μg As L(-1) for MMAA, DMAA, p-ASA, ROX and NIT, respectively. This method exhibited convenient operation, high sensitivity and good repeatability. It was applied to As speciation in different samples including arugula, dog food, dog urine and chicken liver.

  8. A Geant4-based Simulation to Evaluate the Feasibility of Using Nuclear Resonance Fluorescence (NRF) in Determining Atomic Compositions of Body Tissue in Cancer Diagnostics and Irradiation

    Science.gov (United States)

    Gilbo, Yekaterina; Wijesooriya, Krishni; Liyanage, Nilanga

    2017-01-01

    Customarily applied in homeland security for identifying concealed explosives and chemical weapons, NRF (Nuclear Resonance Fluorescence) may have high potential in determining atomic compositions of body tissue. High energy photons incident on a target excite the target nuclei causing characteristic re-emission of resonance photons. As the nuclei of each isotope have well-defined excitation energies, NRF uniquely indicates the isotopic content of the target. NRF radiation corresponding to nuclear isotopes present in the human body is emitted during radiotherapy based on Bremsstrahlung photons generated in a linear electron accelerator. We have developed a Geant4 simulation in order to help assess NRF capabilities in detecting, mapping, and characterizing tumors. We have imported a digital phantom into the simulation using anatomical data linked to known chemical compositions of various tissues. Work is ongoing to implement the University of Virginia's cancer center treatment setup and patient geometry, and to collect and analyze the simulation's physics quantities to evaluate the potential of NRF for medical imaging applications. Preliminary results will be presented.

  9. Solid Phase Extraction of Inorganic Mercury Using 5-Phenylazo-8-hydroxyquinoline and Determination by Cold Vapor Atomic Fluorescence Spectroscopy in Natural Water Samples

    Directory of Open Access Journals (Sweden)

    Mirna Daye

    2013-01-01

    Full Text Available 8-Hydroxyquinoline (8-HQ was chosen as a powerful ligand for Hg solid phase extraction. Among several chelating resins based on 8-HQ, 5-phenylazo-8-hydroxyquinoline (5Ph8HQ is used for mercury extraction in which the adsorption dynamics were fully studied. It has been shown that Hg(II is totally absorbed by 5Ph8HQ within the first 30 minutes of contact time with t1/2 5 minutes, following Langmuir adsorption model. At pH 4, the affinity of mercury is unchallenged by other metals except, for Cu(II, which have shown higher Kd value. With these latter characteristics, 5Ph8HQ was examined for the preconcentration of trace levels of Hg(II. The developed method showed quantitative recoveries of Hg(II with LOD = 0.21 pg mL−1 and RSD = 3–6% using cold vapor atomic fluorescence spectroscopy (CV-AFS with a preconcentration factor greater than 250.

  10. Direct determination of arsenic in soil samples by fast pyrolysis-chemical vapor generation using sodium formate as a reductant followed by nondispersive atomic fluorescence spectrometry

    Science.gov (United States)

    Duan, Xuchuan; Zhang, Jingya; Bu, Fanlong

    2015-09-01

    This new study shows for the first time that sodium formate can react with trace arsenic to form volatile species via fast pyrolysis - chemical vapor generation. We found that the presence of thiourea greatly enhanced the generation efficiency and eliminated the interference of copper. We studied the reaction temperature, the volume of sodium formate, the reaction acidity, and the carried argon rate using nondispersive atomic fluorescence spectrometry. Under optimal conditions of T = 500 °C, the volumes of 30% sodium formate and 10% thiourea were 0.2 ml and 0.05 ml, respectively. The carrier argon rate was 300 ml min- 1 and the detection limit and precision of arsenic were 0.39 ng and 3.25%, respectively. The amount of arsenic in soil can be directly determined by adding trace amount of hydrochloric acid as a decomposition reagent without any sample pretreatment. The method was successfully applied to determine trace amount of arsenic in two soil-certified reference materials (GBW07453 and GBW07450), and the results were found to be in agreement with certified reference values.

  11. Direct determination of arsenic in soil samples by fast pyrolysis–chemical vapor generation using sodium formate as a reductant followed by nondispersive atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Duan, Xuchuan; Zhang, Jingya; Bu, Fanlong

    2015-09-01

    This new study shows for the first time that sodium formate can react with trace arsenic to form volatile species via fast pyrolysis – chemical vapor generation. We found that the presence of thiourea greatly enhanced the generation efficiency and eliminated the interference of copper. We studied the reaction temperature, the volume of sodium formate, the reaction acidity, and the carried argon rate using nondispersive atomic fluorescence spectrometry. Under optimal conditions of T = 500 °C, the volumes of 30% sodium formate and 10% thiourea were 0.2 ml and 0.05 ml, respectively. The carrier argon rate was 300 ml min{sup −1} and the detection limit and precision of arsenic were 0.39 ng and 3.25%, respectively. The amount of arsenic in soil can be directly determined by adding trace amount of hydrochloric acid as a decomposition reagent without any sample pretreatment. The method was successfully applied to determine trace amount of arsenic in two soil-certified reference materials (GBW07453 and GBW07450), and the results were found to be in agreement with certified reference values. - Highlights: • Sodium formate can react with trace arsenic to form volatile species via pyrolysis–chemical vapor generation. • Thiourea can enhance the generation efficiency and eliminate the interference of copper. • Arsenic in soil Sample can be directly determined without sample pretreatment.

  12. Absolute atomic oxygen density measurements for nanosecond-pulsed atmospheric-pressure plasma jets using two-photon absorption laser-induced fluorescence spectroscopy

    Science.gov (United States)

    Jiang, C.; Carter, C.

    2014-12-01

    Nanosecond-pulsed plasma jets that are generated under ambient air conditions and free from confinement of electrodes have become of great interest in recent years due to their promising applications in medicine and dentistry. Reactive oxygen species that are generated by nanosecond-pulsed, room-temperature non-equilibrium He-O2 plasma jets among others are believed to play an important role during the bactericidal or sterilization processes. We report here absolute measurements of atomic oxygen density in a 1 mm-diameter He/(1%)O2 plasma jet at atmospheric pressure using two-photon absorption laser-induced fluorescence spectroscopy. Oxygen number density on the order of 1013 cm-3 was obtained in a 150 ns, 6 kV single-pulsed plasma jet for an axial distance up to 5 mm above the device nozzle. Temporally resolved O density measurements showed that there are two maxima, separated in time by 60-70 µs, and a total pulse duration of 260-300 µs. Electrostatic modeling indicated that there are high-electric-field regions near the nozzle exit that may be responsible for the observed temporal behavior of the O production. Both the field-distribution-based estimation of the time interval for the O number density profile and a pulse-energy-dependence study confirmed that electric-field-dependent, direct and indirect electron-induced processes play important roles for O production.

  13. A comparative evaluation of different ionic liquids for arsenic species separation and determination in wine varietals by liquid chromatography - hydride generation atomic fluorescence spectrometry.

    Science.gov (United States)

    Castro Grijalba, Alexander; Fiorentini, Emiliano F; Martinez, Luis D; Wuilloud, Rodolfo G

    2016-09-02

    The application of different ionic liquids (ILs) as modifiers for chromatographic separation and determination of arsenite [As(III)], arsenate [As(V)], dimethylarsonic acid (DMA) and monomethylarsonic acid (MMA) species in wine samples, by reversed-phase high performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry detection (RP-HPLC-HG-AFS) was studied in this work. Several factors influencing the chromatographic separation of the As species, such as pH of the mobile phase, buffer solution concentration, buffer type, IL concentration and length of alkyl groups in ILs were evaluated. The complete separation of As species was achieved using a C18 column in isocratic mode with a mobile phase composed of 0.5% (v/v) 1-octyl-3-methylimidazolium chloride ([C8mim]Cl) and 5% (v/v) methanol at pH 8.5. A multivariate methodology was used to optimize the variables involved in AFS detection of As species after they were separated by HPLC. The ILs showed remarkable performance for the separation of As species, which was obtained within 18min with a resolution higher than 0.83. The limits of detection for As(III), As(V), MMA and DMA were 0.81, 0.89, 0.62 and 1.00μg As L(-1). The proposed method was applied for As speciation analysis in white and red wine samples originated from different grape varieties.

  14. On-line continuous generation of zinc chelates in the vapor phase by reaction with sodium dithiocarbamates and determination by atomic fluorescence spectrometry

    Science.gov (United States)

    Duan, Xuchuan; Sun, Rui; Fang, Jinliang

    2017-02-01

    The present study shows for the first time that a volatile zinc chelate species can be generated by the on-line continuous merging of an acidified sample solution with an aqueous sodium diethyldithiocarbamate solution followed by rapid separation using a frit-based bubble gas-liquid separator at room temperature. The operating conditions for the generation of the vaporous zinc chelate were preliminarily investigated by non-dispersive atomic fluorescence spectrometry. The possible mechanism of zinc vapor generation is discussed. The study shows that the volatile species is an intermediate species with very similar properties to diethyldithiocarbamic acid and a very short half-life in the acidic solution. Moreover, this species can only be generated by on-line mixing and rapid separation. The efficiency of generation was 33-85% depending on acidity. Under optimal conditions, the flow rates of the sample and Na-DDTC solution were 1.3 ml min- 1, the carrier argon flow rate was 225 ml min- 1, the acid concentration of the sample solution and the concentration of Na-DDTC were 0.05 M and 0.4% (m/v), respectively, the detection limit of zinc was 0.33 (3σ) ng ml- 1, and the relative standard deviation (RSD) was 1.3%. The accuracy of the method was verified by the determination of zinc in the plant reference materials GBW10015 (spinach) and GBW10045 (rice). The results were in good agreement with the certified reference values.

  15. Determination of total Sb,Se Te, and Bi and evaluation of their inorganic species in garlic by hydride-generation-atomic-fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matos Reyes, M.N.; Cervera, M.L.; Guardia, M. de la [University of Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain)

    2009-07-15

    A sensitive and simple analytical method has been developed for determination of Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), Te(VI), and Bi(III) in garlic samples by using hydride-generation-atomic-fluorescence spectrometry (HG-AFS). The method is based on a single extraction of the inorganic species by sonication at room temperature with 1 mol L{sup -1} H{sub 2}SO{sub 4} and washing of the solid phase with 0.1% (w/v) EDTA, followed by measurement of the corresponding hydrides generated under two different experimental conditions directly and after a pre-reduction step. The limit of detection of the method was 0.7 ng g{sup -1} for Sb(III), 1.0 ng g{sup -1} for Sb(V), 1.3 ng g{sup -1} for Se(IV), 1.0 ng g{sup -1} for Se(VI), 1.1 ng g{sup -1} for Te(IV), 0.5 ng g{sup -1} for Te(VI), and 0.9 ng g{sup -1} for Bi(III), in all cases expressed in terms of sample dry weight. (orig.)

  16. Masking Agents Evaluation for Lead Determination by Flow Injection-Hydride Generation-Atomic Fluorescence Spectrometry Technique: Effect of KI, L-Cysteine, and 1,10-Phenanthroline.

    Science.gov (United States)

    Beltrán, Blanca G; Leal, Luz O; Ferrer, Laura; Cerdà, Víctor

    2016-01-01

    Hydride generation (HG) of lead technique presents interferences from foreign ions of complex matrix samples. In order to minimize these interferences, the effect of masking agents such as KI, L-cysteine, and 1,10-phenanthroline was studied in the absence and in the presence of selected interfering species (As, Cr, Cu, and Fe). Different modes of addition of masking agents were accomplished, that is, to either sample or KBH4 reducing solution. The lead determinations were performed using a flow injection analysis (FIA) system coupled to HG and atomic fluorescence spectrometry (AFS). The linearity of calibration curves (1-10 μg Pb L(-1)) was not affected by the addition of the masking agents. The use of KI in the reducing solution diminished interferences from concentrations of As and Cu, while 1,10-phenanthroline showed a positive effect on the interference by As. Moreover, Cr and Cu appeared to be the most serious interfering ions for plumbane (PbH4), because they drastically reduced the analytical signal of lead. Fe did not present any interference under the employed experimental conditions, even at high levels. The accuracy was established through the analysis of certified reference material (i.e., BCR-610, groundwater) using KI as masking agent. The detection limit reached by FIA-HG-AFS proposed methodology was 0.03 μg Pb L(-1).

  17. The analysis of comet mass spectrometric data

    Science.gov (United States)

    Balm, S. P.; Hare, J. P.; Kroto, H. W.

    1991-04-01

    The mass spectra from the Giotto PICCA experiment have been studied using computer simulations based on tabulated mass spectrometric data. It is shown that random mixtures of organic compounds give rise to mass spectra with peaks at about 45, 60, 75, and 90 amu; i.e., separated by about 15 amu. In particular it is shown that the products of Urey-Miller type experiments give mass spectra which can match the observed Giotto data closely. The analysis indicates that the material consists mainly of C/H/O/N (i.e., it is organic), but that the assignment to any well defined organic material is less certain. It is not clear that mass spectrometric studies of complex mixtures have the prospect of yielding this type of information without some form of preseparation.

  18. 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.

  19. Determination of Fe(II) and Fe(III) in small samples by microbore ion chromatography and photometric, atomic absorption spectrometry and total-reflection X-ray fluorescence detection

    Science.gov (United States)

    Sinner, T.; Hoffmann, P.; Ortner, H. M.

    1993-02-01

    Iron(II) and iron(III) are determined after separation on an ion Chromatographie column by various detection systems. "On-line" detection was achieved by the use of a photometer with a flow cell of 0.8 μl; for "off-line" detection, graphite furnace atomic absorption spectrometry or total-reflection X-ray fluorescence were used. The applicability of the methods is shown for standard solutions and atmospheric samples. As a typical result, 50 μg/l of iron can be determined in a 10 μl sample with a nucrobore ion chromatograph-photometer and atomic absorption system and 40 μg/l of iron in a microbore ion chromatograph-total-reflection X-ray fluorescence combination.

  20. Spectrometric Characterization of Active Geosynchronous Satellites

    Science.gov (United States)

    Bedard, D.; Monin, D.; Scott, R.; Wade, G.

    2012-09-01

    Spectrometric characterization of artificial space objects for the purposes of Space Situational Awareness (SSA) has demonstrated great potential since this technique was first reported at this conference over a decade ago. Yet, much scientific work remains to be done before this tool can be used reliably in an operational context. For example, a detailed study of the impacts of a dynamic illumination-object-sensor geometry during individual spectrometric observations has yet to be described. A thorough understanding of this last problem is considered critical if reflectance spectroscopy will be used to characterize active low Earth orbiting spacecraft, in which the Sun-object-sensor geometry varies considerably over the course of a few seconds, or to study space debris that have uncontrolled and varying attitude. It is with the above questions in mind that two observation campaigns were conducted. The first consisted in using small-aperture telescopes to obtain multi-color photometric light curves of active geosynchronous satellites over a wide range of phase angles. The second observation campaign was conducted at the Dominion Astrophysical Observatory (DAO) using the 1.8-metre Plaskett telescope and its Cassegrain spectrograph. The objective of this experiment was to gather time-resolved spectrometric measurements of active geosynchronous satellites as a function of phase angle. This class of satellites was selected because their attitude is controlled and can be estimated to a high level of confidence. This paper presents the two observation campaigns and provides a summary of the key results of this experiment.

  1. Advances in atomic spectroscopy

    CERN Document Server

    Sneddon, J

    1998-01-01

    This volume continues the series'' cutting-edge reviews on developments in this field. Since its invention in the 1920s, electrostatic precipitation has been extensively used in industrial hygiene to remove dust and particulate matter from gases before entering the atmosphere. This combination of electrostatic precipitation is reported upon in the first chapter. Following this, chapter two reviews recent advances in the area of chemical modification in electrothermal atomization. Chapter three consists of a review which deal with advances and uses of electrothermal atomization atomic absorption spectrometry. Flow injection atomic spectroscopy has developed rapidly in recent years and after a general introduction, various aspects of this technique are looked at in chapter four. Finally, in chapter five the use of various spectrometric techniques for the determination of mercury are described.

  2. Hydride Atomic Fluorescence Spectrophotometry Measurement Method of Arsenic and Mercury in Mineral Water%矿泉水中砷和汞的氢化物原子荧光测定法

    Institute of Scientific and Technical Information of China (English)

    韩雪飞

    2016-01-01

    Objective To analyze and determine the hydride atomic fluorescence spectrophotometry measurement method of arsenic and mercury in mineral water. Methods The hydride atomic fluorescence spectrophotometry measurement method was used by means of nitric acid by research staff. Results A certain research showed that the hydride atomic fluorescence spectrophotometry measurement method of arsenic and mercury was conducive to improving the test of materials in mineral water. Conclusion The hydride atomic fluorescence spectrophotometry measurement of arsenic and mercury in mineral water can rapidly conduct a test with relatively accurate results, and it is very suitable for the test work of mineral water, which should be promoted.%目的:分析确定矿泉水中砷和汞的氢化物原子荧光测定的方法。方法研究人员利用化学实验的方法,通过硝酸这个媒介,从而使用氢化物原子荧光测定的形式加以检验的方法。结果通过一定的研究表明,矿泉水中砷和汞的氢化物原子荧光测定法有利于提高对矿泉水中物质的检测。结论矿泉水中砷和汞的氢化物原子荧光测定不仅能够快速地进行检测,而且结果也相对准确,非常适合矿泉水的检验工作,是应该加以推广的方法。

  3. 原子荧光法测透析用水中砷硒锑汞%Atomic fluorescence measuring dialysis water arsenic selenium antimony and mercury

    Institute of Scientific and Technical Information of China (English)

    骆胜超; 李皓

    2011-01-01

    目的:建立透析用水中砷、硒、锑、汞四种微量元素的原子荧光分析法.方法:水中砷和锑加还原剂后同时测定;硒经硝酸高氯酸氧化后,再经盐酸还原后测定;汞直接加硝酸使酸度为5%后测定.结果:汞的检出限为0.024μg/L;硒的检出限为0.044μg/L;砷的检出限为0.011 μg/L;锑的检出限为0.015μg/L.结论:本法用来测定透析用水中极其微量的砷、硒、锑、汞简便快速,且在双道原子荧光法仪中可同时进行砷和锑的检测.%Objective: To establish a method for detection of hemodialysis water arsenic, selenium,antimony and mercury.Methods: Arsenic and antimony in water were detectioned after added reductant, Selenium was detectioned by nitric acid and high chlorine acid oxidationed, Mercury was directly detectioned by adding acidity to 5%. Results:The detect limit for Mercury was 0.024 muon g/L, the detect limit for Selenium was 0. 044 muon g/L, Arsenic detect limit for 0.011 muon g/L, Antimony detect limit to. 015 muon g/L. Conclusion: This method wad simple and rapid for using to determine dialysis water in extremely trace of arsenic and selenium, antimony, mercury, and in double ways for atomic fluorescence analyzer can simultaneously arsenic and antimony detection

  4. Label-Free and Separation-Free Atomic Fluorescence Spectrometry-Based Bioassay: Sensitive Determination of Single-Strand DNA, Protein, and Double-Strand DNA.

    Science.gov (United States)

    Chen, Piaopiao; Wu, Peng; Chen, Junbo; Yang, Peng; Zhang, Xinfeng; Zheng, Chengbin; Hou, Xiandeng

    2016-02-16

    Based on selective and sensitive determination of Hg(2+) released from mercury complex by cold vapor generation (CVG) atomic fluorescence spectrometry (AFS) using SnCl2 as a reductant, a novel label-free and separation-free strategy was proposed for DNA and protein bioassay. To construct the DNA bioassay platform, an Hg(2+)-mediated molecular beacon (hairpin) without labeling but possessing several thymine (T) bases at both ends was employed as the probe. It is well-known that Hg(2+) could trigger the formation of the hairpin structure through T-Hg(2+)-T connection. In the presence of a specific target, the hairpin structure could be broken and the captured Hg(2+) was released. Interestingly, it was found that SnCl2 could selectively reduce only free Hg(2+) to Hg(0) vapor in the presence of T-Hg(2+)-T complex, which could be separated from sample matrices for sensitive AFS detection. Three different types of analyte, namely, single-strand DNA (ssDNA), protein, and double-strand DNA (dsDNA), were investigated as the target analytes. Under the optimized conditions, this bioassay provided high sensitivity for ssDNA, protein, and dsDNA determination with the limits of detection as low as 0.2, 0.08, and 0.3 nM and the linear dynamic ranges of 10-150, 5-175, and 1-250 nM, respectively. The analytical performance for these analytes compares favorably with those by previously reported methods, demonstrating the potential usefulness and versatility of this new AFS-based bioassay. Moreover, the bioassay retains advantages of simplicity, cost-effectiveness, and sensitivity compared to most of the conventional methods.

  5. Determination of thiomersal by flow injection coupled with microwave-assisted photochemical online oxidative decomposition of organic mercury and cold vapor atomic fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Campanella, Beatrice; Onor, Massimo; Mascherpa, Marco Carlo; D’Ulivo, Alessandro [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici-ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Ferrari, Carlo [National Research Council of Italy, C.N.R., Istituto Nazionale di Ottica, INO–UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Bramanti, Emilia, E-mail: bramanti@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Istituto di Chimica dei Composti Organo Metallici-ICCOM-UOS Pisa, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2013-12-04

    Graphical abstract: -- Highlights: •Thiomersal was determined on line using FI-MW/UV-CVGAFS. •MW/UV allows a “green” on line oxidation of organic mercury to Hg{sup II}. •Each measure requires less than 5 min with a LOD of 3 ng mL{sup −1} (as mercury). •Hg concentration in commercial ophthalmic solutions ranges between 7.5 and 59.0 μg mL{sup −1}. -- Abstract: We developed a flow injection (FI) method for the determination of thiomersal (sodium ethylmercurithiosalicylate, C{sub 9}H{sub 9}HgNaO{sub 2}S) based on the UV/microwave (MW) photochemical, online oxidation of organic mercury, followed by cold vapor generation atomic fluorescence spectrometry (CVG-AFS) detection. Thiomersal was quantitatively converted in the MW/UV process to Hg(II), with a yield of 97 ± 3%. This reaction was followed by the reduction of Hg(II) to Hg(0) performed in a knotted reaction coil with NaBH{sub 4} solution, and AFS detection in an Ar/H{sub 2} miniaturized flame. The method was linear in the 0.01–2 μg mL{sup −1} range, with a LOD of 0.003 μg mL{sup −1}. This method has been applied to the determination of thiomersal in ophthalmic solutions, with recoveries ranging between 97% and 101%. We found a mercury concentration in commercial ophthalmic solutions ranging between 7.5 and 59.0 μg mL{sup −1}.

  6. Arsenic fractionation in agricultural soil using an automated three-step sequential extraction method coupled to hydride generation-atomic fluorescence spectrometry.

    Science.gov (United States)

    Rosas-Castor, J M; Portugal, L; Ferrer, L; Guzmán-Mar, J L; Hernández-Ramírez, A; Cerdà, V; Hinojosa-Reyes, L

    2015-05-18

    A fully automated modified three-step BCR flow-through sequential extraction method was developed for the fractionation of the arsenic (As) content from agricultural soil based on a multi-syringe flow injection analysis (MSFIA) system coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS). Critical parameters that affect the performance of the automated system were optimized by exploiting a multivariate approach using a Doehlert design. The validation of the flow-based modified-BCR method was carried out by comparison with the conventional BCR method. Thus, the total As content was determined in the following three fractions: fraction 1 (F1), the acid-soluble or interchangeable fraction; fraction 2 (F2), the reducible fraction; and fraction 3 (F3), the oxidizable fraction. The limits of detection (LOD) were 4.0, 3.4, and 23.6 μg L(-1) for F1, F2, and F3, respectively. A wide working concentration range was obtained for the analysis of each fraction, i.e., 0.013-0.800, 0.011-0.900 and 0.079-1.400 mg L(-1) for F1, F2, and F3, respectively. The precision of the automated MSFIA-HG-AFS system, expressed as the relative standard deviation (RSD), was evaluated for a 200 μg L(-1) As standard solution, and RSD values between 5 and 8% were achieved for the three BCR fractions. The new modified three-step BCR flow-based sequential extraction method was satisfactorily applied for arsenic fractionation in real agricultural soil samples from an arsenic-contaminated mining zone to evaluate its extractability. The frequency of analysis of the proposed method was eight times higher than that of the conventional BCR method (6 vs 48 h), and the kinetics of lixiviation were established for each fraction.

  7. Gold-coated silica as a preconcentration phase for the determination of total dissolved mercury in natural waters using atomic fluorescence spectrometry.

    Science.gov (United States)

    Leopold, Kerstin; Foulkes, Michael; Worsfold, Paul J

    2009-05-01

    A novel solid-phase preconcentration method is reported, using in-house gold-coated silica adsorbent packed in a microcolumn, for the determination of dissolved mercury in natural waters by atomic fluorescence spectrometry (AFS). The adsorbent was prepared by chemical reduction of a Au(III) solution with hydroxylamine in the presence of suspended silica particles. The resulting Au nanoparticles on the silica surface were highly efficient for adsorbing different mercury species from acidified waters without additional reagents. The acidified aqueous samples were passed over the microcolumn, either incorporated in a fully automated flow injection (FI) system directly coupled to the AFS or as part of a portable FI system for in situ preconcentration. After rinsing and drying of the column, Hg(0) was released by heating and directed to the AFS cell for quantification. The method offers significant advantages because no reagents are needed for species conversion, preconcentration, sample storage, or desorption and therefore the risk of contamination is minimized and blank values are lowered. This results in a low detection limit of 180 pg L(-1) using a sample volume of only 7 mL and good reproducibility, with relative standard deviations 90% in spiked river waters (spiked [Hg] = 0, 1, 5, 10 ng L(-1)), and the experimental value for the certified reference material ORMS-4 (elevated mercury in river water) was 22.3 +/- 2.6 ng Hg L(-1) which was in good agreement with the certified value of 22.0 +/- 1.6 ng Hg L(-1) (recovery = 101%). The method was successfully applied to seven different natural waters and wastewaters ([Hg] 0.5-4.6 ng L(-1)) from south west England.

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

    Energy Technology Data Exchange (ETDEWEB)

    Brombach, Christoph-Cornelius [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Chen, Bin; Corns, Warren T. [PS Analytical, Arthur House, Crayfields Industrial Estate, Main Road, Orpington, Kent BR5 3HP (United Kingdom); Feldmann, Jörg [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom); Krupp, Eva M., E-mail: e.krupp@abdn.ac.uk [Trace Element Speciation Laboratory, Department of Chemistry, Meston Walk, University of Aberdeen, Aberdeen AB24 3UE (United Kingdom)

    2015-03-01

    Ultra-traces of methylmercury at the sub-ppt level can be magnified in the foodweb and is of concern. In environmental monitoring a routine robust analytical method is needed to determine methylmercury in water. The development of an analytical method for ultra-trace speciation analysis of methylmercury (MeHg) in water samples is described. The approach is based on HPLC-CV-AFS with on-line preconcentration of water samples up to 200 mL, resulting in a detection limit of 40 pg/L (ppq) for MeHg, expressed as Hg. The unit consists of an optimized preconcentration column filled with a sulfur-based sorption material, on which mercury species are preconcentrated and subsequently eluted, separated and detected via HPLC-CV-AFS (high performance liquid chromatography–cold vapor atomic fluorescence spectrometry). During the method development a type of adsorbate material, the pH dependence, the sample load rate and the carry-over were investigated using breakthrough experiments. The method shows broad pH stability in the range of pH 0 to 7, without the need for buffer addition and shows limited matrix effects so that MeHg is quantitatively recovered from sewage, river and seawater directly in the acidified samples without sample preparation. - Highlights: • We demonstrate that a novel mixture of thiourea-thiolsilica shows an excellent trapping of MeHg between a broad pH range 1–6. • We develop the method so that it can potentially be automated for inorganic and methyl-mercury. • The method is matrix independent with highly accurate results for MeHg in hair CRM extracts and spiked water samples • The limit of detection is around 40 pg/L when just 200 mL sample is used, without any intensive preparation.

  9. New Imaging Spectrometric Method for Rotary Object

    Institute of Scientific and Technical Information of China (English)

    方俊永; 赵达尊; 蒋月娟; 楚建军

    2003-01-01

    A new technique for imaging spectrometer for rotary object based on computed-tomography is proposed. A discrete model of this imaging spectrometric system is established, which is accordant to actual measurements and convenient for computation. In computer simulations with this method, projections of the object are detected by CCD while the object is rotating, and the original spectral images are numerically reconstructed from them by using the algorithm of computed-tomography. Simulation results indicate that the principle of the method is correct and it performs well for both broadband and narrow-band spectral objects.

  10. Arsenic fractionation in agricultural soil using an automated three-step sequential extraction method coupled to hydride generation-atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rosas-Castor, J.M. [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico); Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Portugal, L.; Ferrer, L. [Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Guzmán-Mar, J.L.; Hernández-Ramírez, A. [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico); Cerdà, V. [Group of Analytical Chemistry, Automation and Environment, University of Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca (Spain); Hinojosa-Reyes, L., E-mail: laura.hinojosary@uanl.edu.mx [Universidad Autónoma de Nuevo León, UANL, Facultad de Ciencias Químicas, Cd. Universitaria, San Nicolás de los Garza, Nuevo León, C.P. 66451 Nuevo León (Mexico)

    2015-05-18

    Highlights: • A fully automated flow-based modified-BCR extraction method was developed to evaluate the extractable As of soil. • The MSFIA–HG-AFS system included an UV photo-oxidation step for organic species degradation. • The accuracy and precision of the proposed method were found satisfactory. • The time analysis can be reduced up to eight times by using the proposed flow-based BCR method. • The labile As (F1 + F2) was <50% of total As in soil samples from As-contaminated-mining zones. - Abstract: A fully automated modified three-step BCR flow-through sequential extraction method was developed for the fractionation of the arsenic (As) content from agricultural soil based on a multi-syringe flow injection analysis (MSFIA) system coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS). Critical parameters that affect the performance of the automated system were optimized by exploiting a multivariate approach using a Doehlert design. The validation of the flow-based modified-BCR method was carried out by comparison with the conventional BCR method. Thus, the total As content was determined in the following three fractions: fraction 1 (F1), the acid-soluble or interchangeable fraction; fraction 2 (F2), the reducible fraction; and fraction 3 (F3), the oxidizable fraction. The limits of detection (LOD) were 4.0, 3.4, and 23.6 μg L{sup −1} for F1, F2, and F3, respectively. A wide working concentration range was obtained for the analysis of each fraction, i.e., 0.013–0.800, 0.011–0.900 and 0.079–1.400 mg L{sup −1} for F1, F2, and F3, respectively. The precision of the automated MSFIA–HG-AFS system, expressed as the relative standard deviation (RSD), was evaluated for a 200 μg L{sup −1} As standard solution, and RSD values between 5 and 8% were achieved for the three BCR fractions. The new modified three-step BCR flow-based sequential extraction method was satisfactorily applied for arsenic fractionation in real agricultural

  11. Determination of hydrogen sulfide and volatile thiols in air samples by mercury probe derivatization coupled with liquid chromatography-atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bramanti, Emilia [Italian National Research Council, CNR-Istituto per i Processi Chimico-Fisici, Laboratory of Instrumental Analytical Chemistry, Via G. Moruzzi 1, 56124 Pisa (Italy)]. E-mail: emilia@ipcf.cnr.it; D' Ulivo, Lucia [Italian National Research Council, CNR-Istituto per i Processi Chimico-Fisici, Laboratory of Instrumental Analytical Chemistry, Via G. Moruzzi 1, 56124 Pisa (Italy); Lomonte, Cristina [Italian National Research Council, CNR-Istituto per i Processi Chimico-Fisici, Laboratory of Instrumental Analytical Chemistry, Via G. Moruzzi 1, 56124 Pisa (Italy); Ambiente s.c.r.l., Via Frassina 21, 54033, Carrrara, Massa (Italy); Onor, Massimo [Italian National Research Council, CNR-Istituto per i Processi Chimico-Fisici, Laboratory of Instrumental Analytical Chemistry, Via G. Moruzzi 1, 56124 Pisa (Italy); Zamboni, Roberto [Department of Chemistry and Industrial Chemistry, University of Pisa, Via Risorgimento 35, 56126 Pisa (Italy); Raspi, Giorgio [Italian National Research Council, CNR-Istituto per i Processi Chimico-Fisici, Laboratory of Instrumental Analytical Chemistry, Via G. Moruzzi 1, 56124 Pisa (Italy); D' Ulivo, Alessandro [Italian National Research Council, CNR-Istituto per i Processi Chimico-Fisici, Laboratory of Instrumental Analytical Chemistry, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2006-10-02

    A new procedure is proposed for the sampling and storage of hydrogen sulphide (H{sub 2}S) and volatile thiols (methanethiol or methyl mercaptan, ethanethiol and propanethiol) for their determination by liquid chromatography. The sampling procedure is based on the trapping/pre-concentration of the analytes in alkaline aqueous solution containing an organic mercurial probe p-hydroxymercurybenzoate, HO-Hg-C{sub 6}H{sub 4}-COO{sup -} (PHMB), where they are derivatized to stable PHMB complexes based on mercury-sulfur covalent bonds. PHMB complexes are separated on a C{sub 18} reverse phase column, allowing their determination by liquid chromatography coupled with sequential non-selective UV-vis (DAD) and mercury specific (chemical vapor generation atomic fluorescence spectrometry, CVGAFS) on-line detectors. PHMB complexes, S(PHMB){sub 2}CH{sub 3}S-PHMB, C{sub 2}H{sub 5}S-PHMB and C{sub 3}H{sub 7}S-PHMB, are stable alt least for 12 h at room temperature and for 3 months if stored frozen (-20 deg. C). The best analytical figures of merits in the optimized conditions were obtained by CVGAFS detection, with detection limits (LODc) of 9.7 {mu}g L{sup -1} for H{sub 2}S, 13.7 {mu}g L{sup -1} for CH{sub 3}SH, 17.7 {mu}g L{sup -1} for C{sub 2}H{sub 5}SH and 21.7 {mu}g L{sup -1} for C{sub 3}H{sub 7}SH in the trapping solution in form of RS-PHMB complexes, the relative standard deviation (R.S.D.) ranging between 1.0 and 1.5%, and a linear dynamic range (LDR) between 10 and 9700 {mu}g L{sup -1}. Conventional UV absorbance detectors tuned at 254 nm can be employed as well with comparable R.S.D. and LDR, but with LODc one order of magnitude higher than AFS detector and lower specificity. The sampling procedure followed by LC-DAD-CVGAFS analysis has been validated, as example, for H{sub 2}S determination by a certified gas permeation tube as a source of 3.071 {+-} 0.154 {mu}g min{sup -1} of H{sub 2}S, giving a recovery of 99.8 {+-} 7% and it has been applied to the determination of

  12. Determination of mercury species by the diffusive gradient in thin film technique and liquid chromatography – atomic fluorescence spectrometry after microwave extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pelcová, Pavlína, E-mail: pavlina.pelcova@mendelu.cz; Dočekalová, Hana, E-mail: hana.docekalova@mendelu.cz; Kleckerová, Andrea, E-mail: andrea.kleckerova@mendelu.cz

    2015-03-25

    Highlights: • DGT–MAE–LC–CV-AFS method was developed for determination of four mercury species. • The microwave extraction was used for isolation of mercury species from resin gels. • Optimized DGT–MAE–LC–CV-AFS method provides low detection limits (13–38 ng L{sup −1}). • The diffusion coefficients of four mercury species were simultaneously determined. - Abstract: A diffusive gradient in thin films technique (DGT) was combined with liquid chromatography (LC) and cold vapor atomic fluorescence spectrometry (CV-AFS) for the simultaneous quantification of four mercury species (Hg{sup 2+}, CH{sub 3}Hg{sup +}, C{sub 2}H{sub 5}Hg{sup +}, and C{sub 6}H{sub 5}Hg{sup +}). After diffusion through an agarose diffusive layer, the mercury species were accumulated in resin gels containing thiol-functionalized ion-exchange resins (Duolite GT73, and Ambersep GT74). A microwave-assisted extraction (MAE) in the presence of 6 M HCl and 5 M HCl (55 °C, 15 min) was used for isolation of mercury species from Ambersep and Duolite resin gels, respectively. The extraction efficiency was higher than 95.0% (RSD 3.5%). The mercury species were separated with a mobile phase containing 6.2% methanol + 0.05% 2-mercaptoethanol + 0.02 M ammonium acetate with a stepwise increase of methanol content up to 80% in the 16th min on a Zorbax C18 reverse phase column. The LODs of DGT–MAE–LC–CV-AFS method were 38 ng L{sup −1} for CH{sub 3}Hg{sup +}, 13 ng L{sup −1} for Hg{sup 2+}, 34 ng L{sup −1} for C{sub 2}H{sub 5}Hg{sup +} and 30 ng L{sup −1} for C{sub 6}H{sub 5}Hg{sup +} for 24 h DGT accumulation at 25 °C.

  13. Determination of hydrogen sulfide and volatile thiols in air samples by mercury probe derivatization coupled with liquid chromatography-atomic fluorescence spectrometry.

    Science.gov (United States)

    Bramanti, Emilia; D'Ulivo, Lucia; Lomonte, Cristina; Onor, Massimo; Zamboni, Roberto; Raspi, Giorgio; D'Ulivo, Alessandro

    2006-10-02

    A new procedure is proposed for the sampling and storage of hydrogen sulphide (H2S) and volatile thiols (methanethiol or methyl mercaptan, ethanethiol and propanethiol) for their determination by liquid chromatography. The sampling procedure is based on the trapping/pre-concentration of the analytes in alkaline aqueous solution containing an organic mercurial probe p-hydroxymercurybenzoate, HO-Hg-C6H4-COO- (PHMB), where they are derivatized to stable PHMB complexes based on mercury-sulfur covalent bonds. PHMB complexes are separated on a C18 reverse phase column, allowing their determination by liquid chromatography coupled with sequential non-selective UV-vis (DAD) and mercury specific (chemical vapor generation atomic fluorescence spectrometry, CVGAFS) on-line detectors. PHMB complexes, S(PHMB)2CH3S-PHMB, C2H5S-PHMB and C3H7S-PHMB, are stable alt least for 12 h at room temperature and for 3 months if stored frozen (-20 degrees C). The best analytical figures of merits in the optimized conditions were obtained by CVGAFS detection, with detection limits (LODc) of 9.7 microg L(-1) for H2S, 13.7 microg L(-1) for CH(3)SH, 17.7 microg L(-1) for C2H5SH and 21.7 microg L(-1) for C3H7SH in the trapping solution in form of RS-PHMB complexes, the relative standard deviation (R.S.D.) ranging between 1.0 and 1.5%, and a linear dynamic range (LDR) between 10 and 9700 microg L(-1). Conventional UV absorbance detectors tuned at 254 nm can be employed as well with comparable R.S.D. and LDR, but with LODc one order of magnitude higher than AFS detector and lower specificity. The sampling procedure followed by LC-DAD-CVGAFS analysis has been validated, as example, for H2S determination by a certified gas permeation tube as a source of 3.071+/-0.154 microg min(-1) of H2S, giving a recovery of 99.8+/-7% and it has been applied to the determination of sulfur compounds in real gas samples (biogas and the air of a plant for fractional distillation of crude oil).

  14. Ionic liquid-based zinc oxide nanofluid for vortex assisted liquid liquid microextraction of inorganic mercury in environmental waters prior to cold vapor atomic fluorescence spectroscopic detection.

    Science.gov (United States)

    Amde, Meseret; Liu, Jing-Fu; Tan, Zhi-Qiang; Bekana, Deribachew

    2016-01-01

    Zinc oxide nanofluid (ZnO-NF) based vortex assisted liquid liquid microextraction (ZnO-NF VA-LLME) was developed and employed in extraction of inorganic mercury (Hg(2+)) in environmental water samples, followed by cold vapor atomic fluorescence spectrometry (CV-AFS). Unlike other dispersive liquid liquid microextraction techniques, ZnO-NF VA-LLME is free of volatile organic solvents and dispersive solvent consumption. Analytical signals were obtained without back-extraction from the ZnO-NF phase prior to CV-AFS determination. Some essential parameters of the ZnO-NF VA-LLME and cold vapor generation such as composition and volume of the nanofluid, vortexing time, pH of the sample solution, amount of the chelating agent, ionic strength and matrix interferences have been studied. Under optimal conditions, efficient extraction of 1ng/mL of Hg(2+) in 10mL of sample solution was achieved using 50μL of ZnO-NF. The enrichment factor before dilution, detection limits and limits of quantification of the method were about 190, 0.019 and 0.064ng/mL, respectively. The intra and inter days relative standard deviations (n=8) were found to be 4.6% and 7.8%, respectively, at 1ng/mL spiking level. The accuracy of the current method was also evaluated by the analysis of certified reference materials, and the measured Hg(2+) concentration of GBW08603 (9.6ng/mL) and GBW(E)080392 (8.9ng/mL) agreed well with their certified value (10ng/mL). The method was applied to the analysis of Hg(2+) in effluent, influent, lake and river water samples, with recoveries in the range of 79.8-92.8% and 83.6-106.1% at 1ng/mL and 5ng/mL spiking levels, respectively. Overall, ZnO-NF VA-LLME is fast, simple, cost-effective and environmentally friendly and it can be employed for efficient enrichment of the analyte from various water samples.

  15. Methodology using a portable X-ray fluorescence device for on-site and rapid evaluation of heavy-atom contamination in wounds: a model study for application to plutonium contamination.

    Directory of Open Access Journals (Sweden)

    Hiroshi Yoshii

    Full Text Available Workers decommissioning the Fukushima-Daiichi nuclear power plant damaged from the Great East Japan Earthquake and resulting tsunami are at risk of injury with possible contamination from radioactive heavy atoms including actinides, such as plutonium. We propose a new methodology for on-site and rapid evaluation of heavy-atom contamination in wounds using a portable X-ray fluorescence (XRF device. In the present study, stable lead was used as the model contaminant substitute for radioactive heavy atoms. First, the wound model was developed by placing a liquid blood phantom on an epoxy resin wound phantom contaminated with lead. Next, the correlation between the concentration of contaminant and the XRF peak intensity was formulated considering the thickness of blood exiting the wound. Methods to determine the minimum detection limit (MDL of contaminants at any maximal equivalent dose to the wound by XRF measurement were also established. For example, in this system, at a maximal equivalent dose of 16.5 mSv to the wound and blood thickness of 0.5 mm, the MDL value for lead was 1.2 ppm (3.1 nmol. The radioactivity of 239Pu corresponding to 3.1 nmol is 1.7 kBq, which is lower than the radioactivity of 239Pu contaminating puncture wounds in previous severe accidents. In conclusion, the established methodology could be beneficial for future development of a method to evaluate plutonium contamination in wounds. Highlights: Methodology for evaluation of heavy-atom contamination in a wound was established. A portable X-ray fluorescence device enables on-site, rapid and direct evaluation. This method is expected to be used for evaluation of plutonium contamination in wounds.

  16. Methodology using a portable X-ray fluorescence device for on-site and rapid evaluation of heavy-atom contamination in wounds: a model study for application to plutonium contamination.

    Science.gov (United States)

    Yoshii, Hiroshi; Yanagihara, Kouta; Imaseki, Hitoshi; Hamano, Tsuyoshi; Yamanishi, Hirokuni; Inagaki, Masayo; Sakai, Yasuhiro; Sugiura, Nobuyuki; Kurihara, Osamu; Sakai, Kazuo

    2014-01-01

    Workers decommissioning the Fukushima-Daiichi nuclear power plant damaged from the Great East Japan Earthquake and resulting tsunami are at risk of injury with possible contamination from radioactive heavy atoms including actinides, such as plutonium. We propose a new methodology for on-site and rapid evaluation of heavy-atom contamination in wounds using a portable X-ray fluorescence (XRF) device. In the present study, stable lead was used as the model contaminant substitute for radioactive heavy atoms. First, the wound model was developed by placing a liquid blood phantom on an epoxy resin wound phantom contaminated with lead. Next, the correlation between the concentration of contaminant and the XRF peak intensity was formulated considering the thickness of blood exiting the wound. Methods to determine the minimum detection limit (MDL) of contaminants at any maximal equivalent dose to the wound by XRF measurement were also established. For example, in this system, at a maximal equivalent dose of 16.5 mSv to the wound and blood thickness of 0.5 mm, the MDL value for lead was 1.2 ppm (3.1 nmol). The radioactivity of 239Pu corresponding to 3.1 nmol is 1.7 kBq, which is lower than the radioactivity of 239Pu contaminating puncture wounds in previous severe accidents. In conclusion, the established methodology could be beneficial for future development of a method to evaluate plutonium contamination in wounds. Highlights: Methodology for evaluation of heavy-atom contamination in a wound was established. A portable X-ray fluorescence device enables on-site, rapid and direct evaluation. This method is expected to be used for evaluation of plutonium contamination in wounds.

  17. Evaluation of mass spectrometric techniques for characterization of engineered proteins

    DEFF Research Database (Denmark)

    Roepstorff, P; Schram, K H; Andersen, Jens S.;

    1995-01-01

    Mass spectrometric characterization of engineered proteins has been examined using bovine recombinant Acyl-CoA-Binding Protein (rACBP), [15N]-labeled rACBP, and a number of sequence variants of ACBP produced by site-directed mutagenesis. The mass spectrometric techniques include ESIMS and MALDIMS...... was obtained by LC-ESIMS and by direct mixture analysis by MALDIMS. The latter technique was favorable in terms of sensitivity and speed. A general strategy for mass spectrometric characterization of engineered proteins is suggested....

  18. Mass spectrometric fragmentation pathways of isotope labeled 2,5-disubstituted-1,3,4-oxadiazoles and thiadiazoles

    Science.gov (United States)

    Franski, Rafal; Gierczyk, Blazej; Schroeder, Grzegorz

    2004-01-01

    The mass spectrometric decomposition of protonated, lithiated and methylated (quaternary derivatives) 2-(4'-methoxy)phenyl-5-phenyl-1,3,4-oxadiazoles, containing 13C atom at 5 position of oxadiazole ring as well as its thia correspondent is discussed. The electron-donor properties of C-4' substituent favor cationization of N(3) atom and as a consequence, the losses of HNC(2)O, LiNC(2)O, CH3NC(2)O molecules are favored over HNC(5)O, LiNC(5)O, CH3NC(5)O molecules. Analogous results have been obtained for HNCS and CH3NCS elimination from thiadiazole.

  19. Mercury speciation by high-performance liquid chromatography atomic fluorescence spectrometry using an integrated microwave/UV interface. Optimization of a single step procedure for the simultaneous photo-oxidation of mercury species and photo-generation of Hg0

    Science.gov (United States)

    de Quadros, Daiane P. C.; Campanella, Beatrice; Onor, Massimo; Bramanti, Emilia; Borges, Daniel L. G.; D'Ulivo, Alessandro

    2014-11-01

    We described the hyphenation of photo-induced chemical vapor generation with high performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS) for the quantification of inorganic mercury, methylmercury (MeHg) and ethylmercury (EtHg). In the developed procedure, formic acid in mobile phase was used for the photodecomposition of organomercury compounds and reduction of Hg2 + to mercury vapor under microwave/ultraviolet (MW/UV) irradiation. We optimized the proposed method studying the influence of several operating parameters, including the type of organic acid and its concentration, MW power, composition of HPLC mobile phase and catalytic action of TiO2 nanoparticles. Under the optimized conditions, the limits of detection were 0.15, 0.15 and 0.35 μg L- 1 for inorganic mercury, MeHg and EtHg, respectively. The developed method was validated by determination of the main analytical figures of merit and applied to the analysis of three certified reference materials. The online interfacing of liquid chromatography with photochemical-vapor generation-atomic fluorescence for mercury determination is simple, environmentally friendly, and represents an attractive alternative to the conventional tetrahydroborate (THB) system.

  20. Accurate Atom Counting in Mesoscopic Ensembles

    CERN Document Server

    Hume, D B; Joos, M; Muessel, W; Strobel, H; Oberthaler, M K

    2013-01-01

    Many cold atom experiments rely on precise atom number detection, especially in the context of quantum-enhanced metrology where effects at the single particle level are important. Here, we investigate the limits of atom number counting via resonant fluorescence detection for mesoscopic samples of trapped atoms. We characterize the precision of these fluorescence measurements beginning from the single-atom level up to more than one thousand. By investigating the primary noise sources, we obtain single-atom resolution for atom numbers as high as 1200. This capability is an essential prerequisite for future experiments with highly entangled states of mesoscopic atomic ensembles.

  1. Accurate Atom Counting in Mesoscopic Ensembles

    Science.gov (United States)

    Hume, D. B.; Stroescu, I.; Joos, M.; Muessel, W.; Strobel, H.; Oberthaler, M. K.

    2013-12-01

    Many cold atom experiments rely on precise atom number detection, especially in the context of quantum-enhanced metrology where effects at the single particle level are important. Here, we investigate the limits of atom number counting via resonant fluorescence detection for mesoscopic samples of trapped atoms. We characterize the precision of these fluorescence measurements beginning from the single-atom level up to more than one thousand. By investigating the primary noise sources, we obtain single-atom resolution for atom numbers as high as 1200. This capability is an essential prerequisite for future experiments with highly entangled states of mesoscopic atomic ensembles.

  2. Accurate atom counting in mesoscopic ensembles.

    Science.gov (United States)

    Hume, D B; Stroescu, I; Joos, M; Muessel, W; Strobel, H; Oberthaler, M K

    2013-12-20

    Many cold atom experiments rely on precise atom number detection, especially in the context of quantum-enhanced metrology where effects at the single particle level are important. Here, we investigate the limits of atom number counting via resonant fluorescence detection for mesoscopic samples of trapped atoms. We characterize the precision of these fluorescence measurements beginning from the single-atom level up to more than one thousand. By investigating the primary noise sources, we obtain single-atom resolution for atom numbers as high as 1200. This capability is an essential prerequisite for future experiments with highly entangled states of mesoscopic atomic ensembles.

  3. Analysis of the near-resonant fluorescence spectra of a single rubidium atom localized in a three-dimensional optical lattice

    CERN Document Server

    Kim, Wookrae; Kim, Jung-Ryul; Lee, Yea-Lee; Ihm, Jisoon; An, Kyungwon

    2010-01-01

    Supplementary information is presented on the recent work by W. Kim et al. on the matter-wave-tunneling-induced broadening in the near-resonant spectra of a single rubidium atom localized in a three-dimensional optical lattice in a strong Lamb-Dicke regime.

  4. 离子色谱-氢化物发生原子荧光法测定尿中形态砷%Determination of arsenic species in urine by ion chromatography-hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    魏静; 梁琼; 刘俊娓

    2013-01-01

    Objective:To develop a method for the determination of arsenic species in urine by Ion chromatography - hydride Generation - atomic fluorescence spectrometry. Methods; The urine sample was filtered by 0.45 μm membrane. Using ( NH4 ) 2 HPO4 as mobile phase to explore the best ion chromatographic separation condition and the atomic fluorescence determination condition. The content of various forms of arsenic was determined by Ion chromatography - hydride Generation - atomic fluorescence spectrometry. Results; This method had good relativity and good precision(2.60% ~4. 30% ). The detection limits of As( Ⅲ), DMA, MMA and As( V ) were 2. 0 (μg/L, 4.0 μg/L,4.0 μg/L,8.0 μg/L, the average recoveries of samples were 90.48% ~ 102.90%. Conclusion; The method had the advantages of convenience, speediness, high sensitivity, less interference and high practical value without chemical pretreatment.%目的:建立离子色谱-氢化物发生原子荧光法测定尿中形态砷的方法.方法:尿样经0.45 μm滤膜过滤,以(NH4)2HPO4为流动相,采用离子色谱-氢化物发生原子荧光联机测定不同形态砷的含量.结果:实验结果相关性好,线性范围宽,精密度RSD为2.60%~4.30%,方法检出限为As(Ⅲ)2.0 μg/L,DMA4.0 μg/L,MMA4.0 μg/L,As(V)8.0 μg/L,该方法所得回收率为90.48% ~ 102.90%.结论:方法简便、快速、无需化学预处理、干扰少、灵敏度高,有较高的实用价值.

  5. THE ATOMIC WEIGHTS COMMISSION AND ISOTOPIC ABUNDANCE RATIO DETERMINATIONS.

    Energy Technology Data Exchange (ETDEWEB)

    HOLDEN, N.E.

    2005-08-07

    Following Thomson's discovery of stable isotopes in non-radioactive chemical elements, the derivation of atomic weight values from mass spectrometric measurements of isotopic abundance ratios moved very slowly. Forty years later, only 3 1/2 % of the recommended values were based on mass spectrometric measurements and only 38% in the first half century. It might be noted that two chemical elements (tellurium and mercury) are still based on chemical measurements, where the atomic weight value calculated from the relative isotopic abundance measurement either agrees with the value from the chemical measurement or the atomic weight value calculated from the relative isotopic abundance measurement falls within the uncertainty of the chemical measurement of the atomic weight. Of the 19 chemical elements, whose atomic weight is based on non-corrected relative isotopic abundance measurements, five of these are two isotope systems (indium, iridium, lanthanum, lutetium and tantalum) and one is a three-isotope system (oxygen).

  6. X-ray fluorescence holography

    CERN Document Server

    Hayashi, K; Takahashi, Y

    2003-01-01

    X-ray fluorescence holography (XFH) is a new structural analysis method of determining a 3D atomic arrangement around fluorescing atoms. We developed an XFH apparatus using advanced X-ray techniques and succeeded in obtaining high-quality hologram data. Furthermore, we introduced applications to the structural analysis of a thin film and the environment around dopants and, discussed the quantitative analysis of local lattice distortion. (author)

  7. High performance liquid chromatography coupled to atomic fluorescence spectrometry for the speciation of the hydride and chemical vapour-forming elements As, Se, Sb and Hg: A critical review

    Energy Technology Data Exchange (ETDEWEB)

    Chen Yuwei [Department of Chemistry and Biochemistry, Laurentian University, Ramsey Lake Road, Sudbury P3E 2C6 (Canada); Belzile, Nelson, E-mail: nbelzile@laurentian.ca [Department of Chemistry and Biochemistry, Laurentian University, Ramsey Lake Road, Sudbury P3E 2C6 (Canada); Cooperative Freshwater Ecology Unit, Laurentian University, Ramsey Lake Road, Sudbury P3E 2C6 (Canada)

    2010-06-25

    We present the most recent applications of high performance liquid chromatography (HPLC) hyphenated to hydride generation or chemical vapour generation and atomic fluorescence spectrometry (HG/CVG-AFS), for the determination and speciation of the selected hydride-forming elements arsenic (As), selenium (Se) and antimony (Sb) and the chemical vapour-forming metal Hg. The review focuses on sample preparation, post-column treatments and on the applications of this technique to various liquid and solid samples. This review also intends to discuss some limitations associated to HPLC-HG/CVG-AFS due to the necessity on post-column treatments, including the oxidation of organo-element compounds and the pre-reduction to a suitable valence. Nevertheless, the hyphenated technique HPLC-HG/CVG-AFS remains an efficient, sensitive and affordable approach to perform speciation of the four studied elements as shown by the variety of applications presented and discussed in this review.

  8. 原子荧光光谱法测定四方金矿生活饮用水中砷含量%Determination of arsenic in drinking water Quartet Gold Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    贾书朝; 冯美云

    2014-01-01

    Arsenic is toxic to humans and other organisms carcinogenic effects, due to the toxicity of arsenic large, so the detection of arsenic in water is necessary. Through AFS-230E atomic fluorescence spectrophotometer for determination of arsenic in drinking water to ensure that our guarantee water security.%砷是对人体及其他生物体有毒害作用的致癌物质,由于砷的毒性很大,因此对水质中砷的检测是必要的。本文通过AFS-230E原子荧光分光光度仪对饮用水中砷含量测定,确保我们的保证用水安全。

  9. Synthesis and optimization of fluorescent poly(N-isopropyl acrylamide)-coated surfaces by atom transfer radical polymerization for cell culture and detachment.

    Science.gov (United States)

    Cooperstein, Marta A; Bluestein, Blake M; Canavan, Heather E

    2014-03-16

    Although there are many stimulus-responsive polymers, poly(N-isopropyl acrylamide) (pNIPAM) is of special interest due to the phase change it undergoes in a physiologically relevant temperature range that leads to the release of cells and proteins. The nondestructive release of cells opens up a wide range of applications, including the use of pNIPAM for cell sheet and tissue engineering. In this work, pNIPAM surfaces were generated that can be distinguished from the extracellular matrix. A polymerization technique was adapted that was previously used by Mendez, and the existing protocol was optimized for the culture of mammalian cells. The resulting surfaces were characterized with X-ray photoelectron spectroscopy and goniometry. The developed pNIPAM surfaces were further adapted by incorporation of 5-acrylamidofluorescein to generate fluorescent pNIPAM-coated surfaces. Both types of surfaces (fluorescent and nonfluorescent) sustained cellular attachment and produced cellular detachment of ∼90%, and are therefore suitable for the generation of cell sheets for engineered tissues and other purposes. These surfaces will be useful tools for experiments investigating cellular detachment from pNIPAM and the pNIPAM/cell interface.

  10. Structure determination of adipokinetic hormones using fast atom bombardment tandem mass spectrometry; An unknown adipokinetic hormone (AKH-III) from Locusta migratoria

    Energy Technology Data Exchange (ETDEWEB)

    Heerma, W.; Versluis, C.; Lankhof, H. (Utrecht University (Netherlands). Faculty of Chemistry, Department of Analytical Molecular Spectrometry); Oudejans, R.C.H.M.; Kooiman, F.P.; Beenakkers, A.M.T. (Utrecht University (Netherlands). Department of Experimental Zoology)

    1991-08-01

    Fast atom bombardment mass spectrometry combined with various tandem mass spectrometric techniques and accurate mass measurement were used to elucidate the structure of an unknown biologically active peptide isolated from Locusa migratoria. (author). 23 refs.; 6 figs.; 2 schemes.

  11. Determination of the electromagnetic dipole strength distribution in medium-heavy atomic nuclei by means of nuclear resonance fluorescence; Bestimmung der elektromagnetischen Dipolstaerkeverteilung in mittelschweren Atomkernen mittels Kernresonanzfluoreszenz

    Energy Technology Data Exchange (ETDEWEB)

    Massarczyk, Ralph Jens

    2011-01-17

    During the last hundred years several models were developed to describe the configuration of nuclei. These models have to make predictions, which should be comparable with experiments. As a standard type of experiment the nuclear resonance fluorescence was established. A nucleus is excited by irradiation with photons. By emitting one or more photons the nucleus decays back to the ground state. With this method it is possible to measure energy levels and to determine the strength of their excitation. A continuum of unresolved peaks gives additional strength. The existing setup at the linear electron accelerator ELBE of the Forschungszentrum Dresden-Rossendorf uses bremsstrahlung, produced as a secondary beam in a thin Niobium foil. During the years 2008/09 experiments on the nuclei of {sup 86}Kr and {sup 136}Ba took place there. In this work they will be analyzed. Photon flux and efficiency determination have been done as well as simulations on detector response and non-nuclear scattered background events. For this purpose the GEANT4 package was used. Finally the resulting cross sections were corrected for branching and feeding.

  12. Optimization of the light-induced-fluorescence signals of single atoms and efficient loading of single atoms into a magneto-optical trap%磁光阱中单原子荧光信号的优化及单原子的高效装载

    Institute of Scientific and Technical Information of China (English)

    王杰英; 刘贝; 刁文婷; 靳刚; 何军; 王军民

    2014-01-01

    In our experiment, firstly, we carry out the loading of single atoms in the magneto-optical trap (MOT) by increasing the quadrupole magnetic field gradient, improving the background vacuum, and reducing the diameters of the cooling and trapping laser beams. Secondly, we get the single atomic fluorescence signal of a high signal-to-background ratio in the MOT by means of reducing the detuning of cooling light and increasing its intensity appropriately, and using the polarization spectroscopy locking technique to suppress the fluctuations of cooling laser. In addition, with the real-time feedback on quadrupole magnetic field gradient, we demonstrate a probability of loading single atoms in the MOT as high as 98%. We also measure the statistical properties of the single atomic fluorescence which is excited by continuous light in the MOT;the measured second-order correlation is g(2)(τ =0)=0.09.%实验中首先通过增大四极磁场梯度、提高背景真空度、缩小冷却俘获激光光束直径的方法获得了磁光阱中单原子的装载.其次,通过减小冷却光失谐量、适当增加其光强、同时使用偏振光谱锁频技术抑制冷却光噪声的方法得到了磁光阱中高信号背景比的单原子荧光信号.此外,通过实时反馈控制磁光阱四极磁场梯度的方法,在实验中实现了单原子98%的装载概率.使用Hamburg Brown-Twiss 方案测量了磁光阱中的单原子在连续光激发下所辐射荧光的光子统计特性,得到二阶关联度g(2)(τ=0)=0.09.

  13. Determination of methyl mercury in fish by toluene extraction and atomic fluorescence spectrometry%甲苯萃取-原子荧光光谱法检测鱼肉中甲基汞

    Institute of Scientific and Technical Information of China (English)

    史永富; 田良良; 黄冬梅; 蔡友琼; 黄宣运; 于慧娟

    2014-01-01

    Objective To establish a method for the determination of methyl mercury in fish by toluene extraction and atomic fluorescence spectrometry (AFS). Methods Samples were digested by HBr(48%, v/v) for 30 min, and methyl mercury was extracted by methylbenzene. The extract was back-extracted into aqueous solution by Na2S2O3. The aqueous solution was ready for the analysis by atomic fluorescence spectrometry (AFS). And the present method was used to determine the concentration of methyl mercury in reference materials. Results The result was in accordance with the assigned value. Recoveries were 96.1%and 97.5% respectively. Conclusion The method is effective to determine methyl mercury in fish for its high sensitivity and reproducibility.%目的:建立甲苯萃取-原子荧光光谱检测鱼肉中甲基汞的方法。方法样品经48%氢溴酸水解、甲苯萃取、0.05 mol/L硫代硫酸钠反萃取后,应用AFS-9230原子荧光光谱法进行测定,同时经此前处理后的样品采用DMA-80直接测汞仪进行测定,与原子荧光光谱法的结果进行对比。结果原子荧光光谱法以及直接测汞仪直接测定的结果与标准物质定值吻合,确证该方法的可靠性,适用于鱼、贝等水产品中甲基汞的测定。采用该方法对鱼肉中总汞与甲基汞成分分析标准物质 GBW10029以及英国食品分析水平评估计划(food analysis performance assessment scheme, FAPAS)的罐装鱼肉样品(样品编号07189)进行了检测,检测结果与参考物定值吻合,回收率分别为96.1%,97.5%。结论该方法操作简单,灵敏度高,重现性好,适用于鱼肉中甲基汞含量的定量检测。

  14. Fluorescence spectroscopy

    DEFF Research Database (Denmark)

    Bagatolli, Luis

    2016-01-01

    Fluorescence spectroscopy is a powerful experimental tool used by scientists from many disciplines. During the last decades there have been important developments on distinct fluorescence methods, particularly those related to the study of biological phenomena. This chapter discusses the foundati......Fluorescence spectroscopy is a powerful experimental tool used by scientists from many disciplines. During the last decades there have been important developments on distinct fluorescence methods, particularly those related to the study of biological phenomena. This chapter discusses...

  15. Optimize parameters of hydride generation-atomic fluorescence spectrometry for inorganic arsenic determination in grain%氢化物发生-原子荧光法测定粮食中无机砷条件的研究

    Institute of Scientific and Technical Information of China (English)

    杨庆惠

    2012-01-01

    应用氢化物发生—原子荧光分析技术进行粮食中无机砷测定的研究,通过优化酸度、硼氢化钾、载气流量、灯电流以及原子化器高度等分析条件,结果表明,砷浓度在0~30 ng/ml内呈线性关系,相关系数为0.999 9,相对标准偏差为1.6%,检出限为0.054 μg/L,用此方法测定粮食中无机砷,回收率为96.5%~103.5%.该方法简便、快速、灵敏,在实际样品测定中获得到了满意的结果,便于推广应用.%Hydride generation- atomic fluorescence spectrometry was adopted for determine the inorganic arsenic in grain. The experimental parameters such as Ph, KHB4 concentration, flow rate, lamp current and the height of atomizer were optimized. There is linear relation when the arsenic concentration was between 0~30 ng/ml with a correlation coefficient of 0. 999 9. The relative standard deviation was 1. 6%, and the detection limit was 0. 054μg/L. The recovery rate reached to 96. 5%~103. 5%. This method is simple,rapid and sensitive, and got satisfactory results in practicle,it is worth for generalize.

  16. The Determination of Arsenic in Food Additive Phosphoric Acid by Atomic Fluorescence Spectrometry%原子荧光光谱法测定食品添加剂磷酸中的砷

    Institute of Scientific and Technical Information of China (English)

    陈泉; 邵青松

    2012-01-01

    This paper established the determination of arsenic in food additive phosphoric acid by Atomic fluorescence spectrometry, and the maximum of the relative standard deviation in arsenic test is 3.07%, the recovery rate was 98.7% - 101.2%, the detection limit is 0.09 μg/L; this method is easy operation, rapid, accurate, high sensitivity, worth popularizing in terms of relatively GB3149 -2004 《food additive phosphoric acid》 national standard method for the determination of arsenic.%建立了测定食品添加剂磷酸中砷的原子荧光光谱法,测试中砷的相对标准偏差最高为3.07%,回收率在98.7%-101.2%之间、检出限为0.09μg/L;本法相对GB3149-200k4《食品添加剂磷酸》国家标准中砷的测定方法而言操作简便、快速、准确、灵敏度高,值得推广。

  17. 血液和尿液中砷的原子荧光光度测定法%Determination of arsenic in blood and urine by atom fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    徐燕

    2012-01-01

    [Objective]To explore the optimal method for determining arsenic in blood and urine. [Methods]The determination of arsenic in blood and urine was performed by microwave digest-hydride generation atom fluorescence spectrometry. [Results] Under the optimum condition, the limit of arsenic detection was 0.076 8 jJLg/L; the recoveries were 89.0-103.7% ; RSD was 2.4-5.1%. [Conclusion]The method is simple, rapid, sensitive with less interference and wide linear range.%目的 探讨血液和尿液中砷的最佳测定方法.方法 采用微波消解氢化物发生原子荧光光度法测定血液和尿液中的砷.结果 在最佳条件下砷的最低检出限为0.076 8μg/L,砷回收率为89.0%~103.7%,RSD为2.4 ~5.1%.结论 该方法具有简便,快速,灵敏度高,干扰少,线性范围宽等优点.

  18. Simultaneous determination of arsenic and mercury in polyaluminum chloride by atomic fluorescence spectrometry method%原子荧光光谱法同时测定聚氯化铝中的砷和汞

    Institute of Scientific and Technical Information of China (English)

    秦晓鹏; 吴锴; 陶福棠; 李凯

    2013-01-01

    Application of hydride generation-atomic fluorescence spectrometry method in the simultaneous determination of arsenic and mercury in polyaluminium chloride used for drinking water was studied.This method is of high sensitivity and good accuracy.Under optimal conditions,the potassium borohydride concentration,detection limit,precision,and recovery rate were investigated.Results showed:the detection limits of arsenic and mercury were 0.007 9 μg/L and 0.002 6 g/L, respectively: the recovery rates of arsenic and mercury were 93.75%~103.83% and 105.00%~108.75%, respectively.%研究了应用氢化物发生-原子荧光光谱法同时测定生活饮用水用聚氯化铝中的砷和汞,方法灵敏度高、准确度好在最佳条件下,对硼氢化钾浓度、检出限、精密度、加标回收率等进行了研究.结果表明:方法的检出限砷为0.007 9 μg/L、汞为0.002 6 μg/L,砷、汞的加标回收率分别为93.75%~103.83%和105.00%~ 108.75%.

  19. 氢化物发生-原子荧光光谱法测定红土镍矿中砷%DETERMINATION OF ARSENIC IN LATERITE NICKEL ORES BY HYDRIDE GENERATION-ATOMIC FLUORESCENCE SPECTROMETRY

    Institute of Scientific and Technical Information of China (English)

    陈殿耿; 袁玉霞; 何飞顶

    2012-01-01

    提出了以硫脲-抗坏血酸作为还原掩蔽剂,氢化物发生-原子荧光光谱法( HG-AFS)直接测定红土镍矿中砷的方法.考察了测定的最佳条件、共存元素对测定的影响及方法的精密度和回收率.方法适用于红土镍矿中0.005%~0.1%砷的测定.%A method for the determination of arsenic in laterite nickel ores by hydride generation-atomic fluorescence spectrometry (HG-AFS) directly with thiourea-ascorbic acid hydrochloride as masking is proposed. The optimum experimental parameters, the effect of coexistent elements on the determination of arsenic, the precision and recovery of the method are investigated. The method can be applied to the determination of 0. 005% ~ 0. 1% arsenic in laterite nickel ores.

  20. 原子荧光光谱仪测定底泥中砷含量的不确定度评定%The Uncertainty Assessment of Measuring the Arsenic Content in Sludge with Atomic Fluorescence Spectrometer

    Institute of Scientific and Technical Information of China (English)

    张俊

    2012-01-01

    This article introduces the uncertainty assessment in measuring the arsenic content in sludge with the atomic fluorescence spectrometer. The factors of uncertainty during the measurement are analyzed and identified. It presents a relatively comprehensive assessment of measurement uncertainty. According to the standard uncertainty of least squares method fitting calculation working curve, the standard uncertainty resulted from less measurements is assessed with the range method.%介绍了原子荧光光谱仪测定底泥中砷含量的不确定度评定方法,分析和识别测量过程中不确定度的来源,较为全面地评定了测量不确定度。根据最小二乘法拟合计算工作曲线的标准不确定度,采用极差法评定测量次数较少时引起的标准不确定度。

  1. Solute and solvent dynamics in confined equal-sized aqueous environments of charged and neutral reverse micelles: a combined dynamic fluorescence and all-atom molecular dynamics simulation study.

    Science.gov (United States)

    Guchhait, Biswajit; Biswas, Ranjit; Ghorai, Pradip K

    2013-03-28

    Here a combined dynamic fluorescence and all-atom molecular dynamics simulation study of aqueous pool-size dependent solvation energy and rotational relaxations of a neutral dipolar solute, C153, trapped in AOT (charged) and IGPAL (neutral) reverse micelles (RMs) at 298 K, is described. RMs in simulations have been represented by a reduced model where SPC/E water molecules interact with a trapped C153 that possesses realistic charge distributions for both ground and excited states. In large aqueous pools, measured average solvation and rotation rates are smaller for the neutral RMs than those in charged ones. Interestingly, while the measured average solvation and rotation rates increase with pool size for the charged RMs, the average rotation rates for the neutral RMs exhibit a reverse dependence. Simulations have qualitatively reproduced this experimental trend and suggested interfacial location for the solute for all cases. The origin for the subnanosecond Stokes shift dynamics has been investigated and solute-interface interaction contribution quantified. Simulated layer-wise translational and rotational diffusions of water molecules re-examine the validity of the core-shell model and provide a resolution to a debate regarding the origin of the subnanosecond solvation component in dynamic Stokes shift measurements with aqueous RMs but not detected in ultrafast IR measurements.

  2. 硼氢化钾还原冷原子荧光测定大米中的汞%Determination of mercury in rice by potassium borohydride reduction cold vapor atomic fluorescence

    Institute of Scientific and Technical Information of China (English)

    毛荐; 刘忠胜

    2011-01-01

    本方法采用硝酸-过氧化氢微波消解,硼氢化钾还原冷原子荧光测定大米中的汞,消解液无需赶酸,直接测汞,方法简便快捷,实验检出限浓度为0.024μg/L,线性范围0~40 ng/ml,经国家一级标准物质验证,方法准确可靠。%This method uses nitric acid-hydrogen peroxide microwave digestion,potassium borohydride reduction of rice in cold vapor atomic fluorescence of mercury,acid digestion solution without the need to catch,direct measurement of mercury,the method is quick and easy experimental detection limit concentration of 0.024 μg / L,the linear range of 0 ~ 40 ng / ml,The method is accurate and reliable verified by the national standard.

  3. 浅谈原子荧光法对测定工业污水中砷%Discussion on the Atomic Fluorescence Method for Determination of Arsenic in Industrial Waste Water

    Institute of Scientific and Technical Information of China (English)

    曾正强; 向黎黎; 姚太平

    2012-01-01

    Arsenic widely existed in the nature as a kind of very toxic elements. The main source of arsenic was the in- dustrial sewage discharged from the mining and metallurgical, chemical, pharmaceutical, textile, glass and leather manufac- turing production department, the determination of arsenic was routine laboratory item of water quality monitoring, the deter- mination of arsenic in water was summerized by the method of hydride generation - atomic fluorescence spectrometry.%砷元素作为一种毒性非常大的元素广泛的存在于自然界中。砷的主要来源是采矿冶金、化工、制药、纺织、玻璃和皮革制造等生产部门产生的工业污水,砷元素的测定是水质监测中的常规化验项目,本文对采用氢化物发生-原子荧光法测定水中的砷进行了概述。

  4. A simple and sensitive flow-injection on-line preconcentration coupled with hydride generation atomic fluorescence spectrometry for the determination of ultra-trace lead in water, wine, and rice.

    Science.gov (United States)

    Wu, Hong; Jin, Yan; Luo, Mingbiao; Bi, Shuping

    2007-09-01

    A simple and sensitive flow-injection on-line separation and preconcentration system coupled to hydride generation atomic fluorescence spectrometry (HG-AFS) was developed for ultra-trace lead determination in water, wine, and rice samples, with the salient advantages of its minimization of transition-metal interferences and tolerance to an ethanol matrix. A lead hydroxide precipitate was achieved by the on-line merging of a sample and an ammonium buffer solution and collected onto the inner walls of a knotted reactor (KR). Removal of the residual solution from KR was achieved by air flow, and dissolution of the precipitate was carried out by using 0.2 mol l(-1) HCl. With a sample consumption of 11.7 ml, an enhancement factor of 16 was obtained at a sample throughput of 30 h(-1). The limit of detection (3s) was 16 ng l(-1) and the precision (RSD) for 1.0 microg l(-1) Pb was 3.4%.

  5. Ultraviolet irradiation-induced substitution of fluorine with hydroxyl radical for mass spectrometric analysis of perfluorooctane sulfonyl fluoride.

    Science.gov (United States)

    Wang, Peng; Tang, Xuemei; Huang, Lulu; Kang, Jie; Zhong, Hongying

    2016-01-28

    A rapid and solvent free substitution reaction of a fluorine atom in perfluorooctane sulfonyl fluoride (PFOSF) with a hydroxyl radical is reported. Under irradiation of ultraviolet laser on semiconductor nanoparticles or metal surfaces, hydroxyl radicals can be generated through hole oxidization. Among all fluorine atoms of PFOSF, highly active hydroxyl radicals specifically substitute the fluorine of sulfonyl fluoride functional group. Resultant perfluorooctane sulfonic acid is further ionized through capture of photo-generated electrons that switch the neutral molecules to negatively charged odd electron hypervalent ions. The unpaired electron subsequently initiates α O-H bond cleavage and produces perfluorooctane sulfonate negative ions. Hydroxyl radical substitution and molecular dissociation of PFOSF have been confirmed by masses with high accuracy and resolution. It has been applied to direct mass spectrometric imaging of PFOSF adsorbed on surfaces of plant leaves.

  6. Absorption spectrum, mass spectrometric properties, and electronic structure of 1,2-benzoquinone.

    Science.gov (United States)

    Albarran, Guadalupe; Boggess, William; Rassolov, Vitaly; Schuler, Robert H

    2010-07-22

    Absorption spectrophotometric and mass spectrometric properties of 1,2-benzoquinone, prepared in aqueous solution by the hexachloroiridate(IV) oxidation of catechol and isolated by HPLC, are reported. Its absorption spectrum has a broad moderately intense band in the near UV with an extinction coefficient of 1370 M(-1)cm(-1) at its 389 nm maximum. The oscillator strength of this band contrasts with those of the order-of-magnitude stronger approximately 250 nm bands of most 1,4-benzoquinones. Gaussian analysis of its absorption spectrum indicates that it also has modestly intense higher energy bands in the 250-320 nm region. In atmospheric pressure mass spectrometric studies 1,2-benzoquinone exhibits very strong positive and negative mass 109 signals that result from the addition of protons and hydride ions in APCI and ESI ion sources. It is suggested that the hydride adduct is formed as the result of the highly polar character of ortho-quinone. On energetic collision the hydride adduct loses an H atom to produce the 1,2-benzosemiquinone radical anion. The present studies also show that atmospheric pressure mass spectral patterns observed for catechol are dominated by signals of 1,2-benzoquinone resulting from oxidation of catechol in the ion sources. Computational studies of the electronic structures of 1,2-benzoquinone, its proton and hydride ion adducts, and 1,2-benzosemiquinone radical anion are reported. These computational studies show that the structures of the proton and hydride adducts are similar and indicate that the hydride adduct is the proton adduct of a doubly negatively charged 1,2-benzoquinone. The contrast between the properties of 1,2- and 1,4-benzoquinone provides the basis for considerations on the effects of conjugation in aromatic systems.

  7. 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.

  8. Precise timing of the last interglacial period from mass spectrometric determination of thorium-230 in corals

    Science.gov (United States)

    Chen, J. H.; Wasserburg, G. J.; Ku, T.-L.; Edwards, R. Lawrence

    1987-01-01

    The development of mass spectrometric techniques for determination of Th-230 abundance has made it possible to reduce analytical errors in (U-238)-(U-234)-(Th-230) dating of corals even with very small samples. Samples of 6 x 10 to the 8th atoms of Th-230 can be measured to an accuracy of + or - 3 percent (2sigma), and 3 x 10 to the 10th atoms of Th-230 can be measured to an accuracy of + or - 0.2 percent. The time range over which useful age data on corals can be obtained now ranges from about 50 to about 500,000 years. For young corals, this approach may be preferable to C-14 dating. The precision with which the age of a coral can now be determined should make it possible to critically test the Milankovitch hypothesis concerning Pleistocene climate fluctuations. Analyses of a number of corals that grew during the last interglacial period yield ages of 122,000 to 130,000 years. The ages coincide with, or slightly post-date, the summer solar insolation high at 65 deg N latitude which occurred 128,000 years ago. This supports the idea that changes in Pleistocene climate can be the result of variations in the distribution of solar insolation caused by changes in the geometry of the earth's orbit and rotation axis.

  9. Inductively coupled plasma atomic emission spectrometric determination of acid-soluble metal elements chromium,manganese, zinc and copper in talcum powder%电感耦合等离子体原子发射光谱法测定滑石粉中酸溶金属元素铬锰锌铜

    Institute of Scientific and Technical Information of China (English)

    胡晓静; 曾泽; 王长文; 仇薪越; 牟明仁; 富瑶; 沈桂玲; 刘向宽

    2011-01-01

    After digestion by aqua regia with microwave and selection of corresponding spectral lines at 267. 7, 257. 6, 213. 8 and 324. 7 nm as analytical lines, the acid-dissoluble metal elements including chromium, manganese, zinc and copper in talcum powder were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) under optimized conditions with radio frequency power of 1 250 W, auxiliary air flow rate of 0. 60 L/min and atomizer pressure of 26 psi. When the concentration of each testing element was 2. 0 μg/mL, the interferences caused by 20. 0 μg/mL of I-ron, magnesium, calcium, aluminum, zinc, nickel and copper were all less than 5 %. Since the contents of these elements in talcum powder were less than 1 %, their influence on the determination could be ignored. The detection limits of chromium, manganese, zinc and copper were 0. 004 8, 0. 003 8, 0. 001 and 0. 002 6 μg/mL, respectively. This proposed method was applied in actual samples, and the determination results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) with relative standard deviations (RSD, n = 8) of 1.1%-4. 2% and recoveries of 93 %-107 %.%以王水作溶剂,微波消解法消解样品,选择267.7、257.6、213.8和324.7 nm波长的光谱线分别作为铬、锰、锌和铜的分析线,在发射功率为1 250 W、辅助气流量为0.60 L/min、雾化器压力为26 psi的优化条件下以电感耦合等离子体原子发射光谱法(ICP-AES)测定了滑石粉中酸溶金属元素铬、锰、锌、铜含量.样品中的基体组分硅酸镁在王水中的溶解量很少,对测定没有影响.当测定待测元素浓度均为2.0μg/mL的溶液时,20.0 μg/mL的铁、镁、钙、铝、锌、镍、铜对待测元素的干扰均小于5%.由于滑石粉中这些元素含量小于1%,因此它们对测定的影响可以忽略.铬、锰、锌、铜的检出限分别为0.004 8、0.003 8、0.001、0.002 6μg/mL.滑石粉样品分析

  10. 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.

  11. 氢化物发生-原子荧光光谱法测定Inconel 718合金中痕量硒%Determination of trace selenium in 718 alloy by hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    向祥蓉; 刘虹; 王佼

    2012-01-01

    本文采用氢化物发生-原子荧光光谱法测定Inconel718合金中痕量硒.对影响其测定的负高压、灯电流、载气流量、屏蔽气流量、载流酸类酸度、硼氢化钾等因素进行了较为详细的研究,优化了测定条件,考察了Inconel718合金主要组成元素和基体元素对硒测定的影响.结果表明,用氟化氨溶液络合,柠檬酸溶液作干扰抑制剂能基本消除基体元素和主要组成元素的干扰.硒浓度在0~100μg/L与荧光强度有良好的线性关系,方法的检出限为0.0083μg/L.对铁镍基高温合金标准样品和Inconel 718合金样品进行9次测定,相对标准偏差为1.6%~3.5%.%In this paper a simple and fast analytical procedure for the determination of selenium in Inconel 718 alloy by hydride generation atomic fluorescence spectrometry(HG-AFS) was developed. The in fluence of instrument parameters such as voltage of PMT, current of lamp, atomizer height, carrier gas rate,shield gas rate and concentration of HCI and KBH4 on the determination of selenium were studied, and the optimized conditions were obtained. Interference of coexistent elements and methods to eliminate the interference were investigated in detail. The results showed that ammonium fluoride and citric acid mo nohydrate were the best masking. Under the optimized conditions, the linear range of selenium is 0 ~ 100μg/L, and the detection limit is 0. 0083 μg/L. The relative standard deviation is 1. 6%~3. 5%(n=9) for the standard sample and the sample of Inconel 718 alloy.

  12. Determination of arsenic and mercury in the rice by microwave digestion-atomic fluorescence spectrometry%大米中砷和汞的微波消解-原子荧光光谱测定法

    Institute of Scientific and Technical Information of China (English)

    李树雄; 张荣

    2012-01-01

    目的 建立双道原子荧光光谱法同时测定大米中的砷和汞的方法.方法 采用微波消解法处理大米样品,以原子荧光光谱法同时测定其中的砷和汞.结果 砷和汞的检出限分别为0.0044、0.039 μg/L;砷、汞标准溶液分别在1.0 ~20.0和0.10 ~1.20 μg/L范围内线性良好,其相关系数分别为0.9995、0.9992;精密度RSD:测定含2.0 μg/L砷和0.4 μg/L汞的混合标准溶液的RSD分别为2.12% 、4.59%.样品加标回收率:砷92.2% ~96.8%,汞90.3% ~92.1%.结论 该方法灵敏度、准确度高,操作方便快速,具有较低的检出限,能满足同时测定大米中砷和汞含量的测定工作.%[Objective ] To establish the method for simultaneous determination of trace arsenic and mercury in rice by dual-channel atomic fluorescence spectrometry. [Methods] The rice samples was digested by microwave, then the trace arsenic and mercury were simultaneously determined by Atomic fluorescence spectrometry. [ Results] The detection limits were 0.004 4 (μg/L for arsenic and 0.039 (μg/L for mercury; there was a linear relationship between 1.0-20.0 μg/L of arsenic standard solution, 0.10-1.20 (μg/L of mercury standard solution. The correlation coefficients were 0.999 5 for arsenic and 0.999 2 for mercury. The precision RSD was 2.12% for 2.0 μg/L arsenic mixed standard solution, and 4.59% for 0.4 μg/L mercury mixed standard solution. The recoveries were 92.2%-96.8% for arsenic and 90.3%-92.1% for mercury. [Conclusion]This method is very sensitive, with high accuracy, easy and fast. It has lower detecting limit, and can determine the content of Arsenic and Mercury in rice simultaneously

  13. 氢化物发生原子荧光光谱法测量化妆品中Sb的价态%Valent speciation analysis of antimony in cosmetics by hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    肖融; 张新智; 王昌钊; 冯礼; 秦德元; 刘霁欣

    2012-01-01

    考察了NaF、8-羟基喹啉、柠檬酸对Sb(Ⅲ)和Sb(V)原子荧光信号的掩蔽作用和还原解柠檬酸除掩蔽作用的方法.结果表明,0.10mol/L柠檬酸对Sb(V)掩蔽作用最强,且对Sb(Ⅲ)有增敏作用,最适于作为Sb价态测量的掩蔽剂,而10g/L碘化钾(KI)+ 10g/L硫脲(Tu)可在5h内完全解除柠檬酸对Sb(V)的掩蔽作用.据此建立了化妆品中Sb价态的非色谱氢化物发生原子荧光测量方法.样品经0.10mol/L柠檬酸提取两次后,离心去上清液,合并定容,得到提取液;提取液酸化后直接测得Sb(Ⅲ)含量;提取液酸化并加入KI+Tu,放置5h以上后可测得Sb(V)与Sb(Ⅲ)的含量和,此值减去Sb(Ⅲ)含量可得Sb(V)含量.计算表明,该方法对Sb(Ⅲ)和Sb(V)的检出限(3σ)均为0.32μg/L,定量限(3σ)均为1.0μg/L.对实际化妆品作了测量,Sb(Ⅲ)和Sb(V)的加标回收率在70%~130%之间.实验中存在少量Sb(Ⅲ)到Sb(V)的转化.%The masking effects of NaF, 8-hydroxygquinoline and citric acid on the atomic fluorescence signals of Sb(Ⅲ ) and Sb( V ) And the method for eliminating the masking effect of citric acid were investigated. The results show that 0. 10 mol/L citric acid has the strongest masking effect on Sb(V) and can increase the sensitivity of Sb(Ⅲ) , and l0g/L KI+l0g/L thiourea can completely eliminate the masking effect of citric acid in >5h. Based on this, a method for analyzing the valent speciation of Sb in cosmetics by hydride generation atomic fluorescence spectrometry (HGAFS) was developed. The samples were extracted twice with 0. L0ml/L citric acid. The supernatant was removed by centrifugation and the residues were merged asextract solution. After the acidification of the extract solution, the Sb(Ⅲ) content was determined directly. Then the extract solution was added with KI (10g/L)+ thiourea (l0g/L) and set aside for >5h before the total content of Sb(V) and Sb(Ⅲ) was determined. The Sb( V) content was obtained by subtracting Sb

  14. Simultaneous speciation of inorganic arsenic and antimony in water samples by hydride generation-double channel atomic fluorescence spectrometry with on-line solid-phase extraction using single-walled carbon nanotubes micro-column

    Energy Technology Data Exchange (ETDEWEB)

    Wu Hong, E-mail: wuhong1968@hotmail.com; Wang Xuecui; Liu Bing; Liu Yueling; Li Shanshan; Lu Jusheng; Tian Jiuying; Zhao Wenfeng; Yang Zonghui

    2011-01-15

    A new method was developed for the simultaneous speciation of inorganic arsenic and antimony in water by on-line solid-phase extraction coupled with hydride generation-double channel atomic fluorescence spectrometry (HG-DC-AFS). The speciation scheme involved the on-line formation and retention of the ammonium pyrrolidine dithiocarbamate complexes of As(III) and Sb(III) on a single-walled carbon nanotubes packed micro-column, followed by on-line elution and simultaneous detection of As(III) and Sb(III) by HG-DC-AFS; the total As and total Sb were determined by the same protocol after As(V) and Sb(V) were reduced by thiourea, with As(V) and Sb(V) concentrations obtained by subtraction. Various experimental parameters affecting the on-line solid-phase extraction and determination of the analytes species have been investigated in detail. With 180 s preconcentration time, the enrichment factors were found to be 25.4 for As(III) and 24.6 for Sb(III), with the limits of detection (LODs) of 3.8 ng L{sup -1} for As(III) and 2.1 ng L{sup -1} for Sb(III). The precisions (RSD) for five replicate measurements of 0.5 {mu}g L{sup -1} of As(III) and 0.2 {mu}g L{sup -1} of Sb(III) were 4.2 and 4.8%, respectively. The developed method was validated by the analysis of standard reference materials (NIST SRM 1640a), and was applied to the speciation of inorganic As and Sb in natural water samples.

  15. Simultaneous Determination of Arsenic and Antimony in Water by Hydride Generation-Atomic Fluorescence Spectrometry%氢化物发生-原子荧光光谱法同时测定水中砷和锑

    Institute of Scientific and Technical Information of China (English)

    黄选忠; 万忠卫; 杜宏山; 郑丽

    2013-01-01

    建立在硝酸介质中用氢化物发生-原子荧光光谱法同时测定水中砷和锑的方法。优化了仪器工作条件、酸度、硼氢化钾及还原剂浓度。砷、锑的线性范围为0~10.0µg/L;检出限分别为0.02,0.01µg/L;测定结果的相对标准偏差分别为1.77%~3.72%,2.95%~4.87%(n=6);加标回收率分别为98%~106%,96%~105%。该法操作简便,灵敏度高,快速,便于推广,适用于水中砷和锑的同时测定。%The method for simultaneous determination of arsenic and antimony in water was established by hydride-generation atomic fluorescence spectrometry in nitric acid medium. Instrument condition,acidity,concentration of potassium borohydride and thiourea-ascorbic acid were selected. The linear relationship of arsenic and antimony was 0-10.0 µg/L. The detection limit of arsenic and antimony was 0.02 µg/L and 0.01 µg/L, the relative standard deviation of arsenic and antimony determination results was 1.77%-3.72%and 2.95%-4.87%(n=6) , the recovery of standard addition of arsenic and antimony was 98%-106%and 96%-105%respectively. This method has the advantages of simple operation and high sensitivity,it is rapid and easy to spread,which is suitable for simultaneous determination of arsenic and antimony in water.

  16. Optimization of Atomic Fluorescence Determination of Arsenic and Mercury in Leather%原子荧光光谱法测定皮革中砷和汞的条件优化

    Institute of Scientific and Technical Information of China (English)

    余红

    2012-01-01

    用硝酸、过氧化氢微波消解处理皮革样品,获得均匀的样品消解液。用原子荧光光谱法测定皮革中的砷和汞,并优化了测定条件。砷的相对标准偏差≤3.8%,方法检出限为0.0376μg/L,回收率为97.8%~102.8%;汞的相对标准偏差为≤7.2%,方法检出限为0.0046μg/L,回收率为95.0%-103.0%。%A uniform leather sample digestion solution was obtained firstly with the microwave digestion treatment method using nitric acid and hydrogen peroxide, and then the conditions for detecting Arsenic and Mercury in leather using atomic fluorescence method were optimized. The results indicated that the relative standard deviation was not greater than 3.8%, the detection limit was 0.0376 μg/L, the recovery rate was 97.8%-102.8% for Arsenic; and the relative standard deviation was not greater than 7.2%, the detection limit was 0.0046 μg/L, the recovery rate was 95.0%-103.0% for Mercury.

  17. Determination of arsenic and hydrargyrum in cosmetics by using Hydride atomic fluorescence spectroscopy%氢化物原子荧光光谱法测化妆品中的砷、汞

    Institute of Scientific and Technical Information of China (English)

    李淑娜

    2012-01-01

    目的:建立化妆品中准确测定砷、汞的测定方法.方法:采用HNO3-H2SO4混合酸消化化妆品、氢化物发生原子荧光光谱法测定砷、汞的含量.结果:砷的方法检出限为0.0227 μg/g,测定精密度为0.9%~1.4%,回收率为96.0% ~ 102.7%,汞的方法检出限为0.171 ng/g,测定精密度为1.4% ~2.0%,回收率为90.0% ~ 105.0%.结论:该方法精密度好,回收率及灵敏度高,线性范围宽,可作为化妆品中微量砷、汞的测定方法.%Objective: To establish the method for accurate determination of arsenic and hydrargyrum in cosmetics. Methods: The contents of arsenic and hydrargyrum were determined by using mixed acid H2SO4 - HNO3 digestion cosmetics and hydride generation atomic fluorescence spectroscopy. Results: The detection limit of arsenic was 0.0227 μg/g, the measuring precision was 0.9% ~ 1.4% , and the recovery rate was 96.0% ~ 102. 7% . The detection limit of hydrargyrum was 0. 171 ng/g, the measuring precision was 1.4% ~2.0%, and the recovery rate was 90. 0% ~105.0%. Conclusion; The method could be used to determine the trace arsenic and hydrargyrum in cosmetics, with good precision, high recovery rate and sensitivity and wide linear range.

  18. Analysis of Selenium in Blood of Patients with Lung Cancer by Microwave Digestion-Atomic Fluorescence Spectrometry%微波消解-原子荧光光谱法分析肺癌患者全血中硒

    Institute of Scientific and Technical Information of China (English)

    董琳; 张欣欣; 王继灵; 吴桂平; 杨庆斌

    2014-01-01

    目的:探讨肺癌患者血样中硒含量的变化。方法采集肺癌组和对照组血样,用硝酸、过氧化氢混合液微波消解样品,采用原子荧光光谱法测定血样中硒的含量。结果肺癌组和对照组硒平均质量浓度分别为0.087、0.123 mg/L。结论肺癌患者血样硒含量明显降低,缺硒可能是导致肺癌高发的重要因素。%Objective The paper investigates the change of the selenium content in the blood samples of patients with lung cancer .Methods The writer applies miscible liquids of nitric acid and hydrogen peroxide to the digestion of the collected blood samples from lung cancer group and the control group , using atomic fluorescence spectrometry to determine the content of selenium in blood samples .Results The average content of selenium in the lung cancer group and control group in average content of selenium are 0.087 mg/L and 0.123 mg/L respectively .Conclusion The content of selenium significantly lowered in the blood samples collected from patients with lung cancer .Selenium deficiency may be an important factor leading to high incidence of lung cancer .

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

    Science.gov (United States)

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

    2005-10-31

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

  20. Determination of trace germanium in health protection food by hydride generation atomic fluorescence spectrometry%氢化物-原子荧光光谱法测定保健食品中痕量锗

    Institute of Scientific and Technical Information of China (English)

    宋伟明; 倪刚; 胡奇林; 全晓塞

    2001-01-01

    A new method was introduced for the determination of trace germanium by hydride generation atomic fluorescence spectrometry(HGAFS).The effect of the medium amounts of acid, action of hydride and screening agent of the determination of germanium was investigated. The operating condition of the instrument was optimized. The interference from foreign ions was eliminated by adding phosphoric acid and tartaric acid. This method was applied to the determination of germanium in some health protection and nourishing food. The detection limit (3δ) is 6.2 ng/g with a RSD of 5% .The recovery of standard addition is in 95%~105%.%提出了以氢化物-原子荧光光谱法测定保健食品中锗的新方法,研究了酸介质、氢化物发生、增敏掩蔽剂等因素对测定的影响,并选择出仪器的最佳工作条件;采用磷酸-酒石酸介质进行测定,不但可有效消除共存离子的干扰,而且起到增敏作用,方法的检出限为6.2,ng/g,相对标准偏差(RSD)在5%以内,加标回收率为95%~105%,结果令人满意.

  1. Determination of Se in Saffron by Using Hydride Generation Atomic Fluorescence Spectrometry%氢化物发生原子荧光光谱法测定西红花柱头中的硒

    Institute of Scientific and Technical Information of China (English)

    张宏; 张新申; 颜钫; 陈放

    2001-01-01

    A method for determination of Se in saffron using AFS-230 hydride generation atomic fluorescence spectrometry was introduced.Detections were completed made in every possible best condition.The optimal analytical conditions in HClO4-HNO3 were examined.The detection limit is 0.5μg/L.The linear range is 1.5~15.0 μg/L.The correlation coefficient is 0.9999,and the recovery rate is about 90%~97%.Se of saffrons from 4 regions was determined by standard curve method.The experiment results show that this method has low detection limit,high accurate,simple operation,fast and low cost.It's easy to be spread.%应用AFS-230型双道原子荧光光谱计进行了氢化物发生原子荧光光谱法测定西红花柱头中硒的研究,方法中采用硝酸做介质,并对各种最佳分析条件进行了测定。线性范围为1.5~15μg/L,相关系数R=0.9999,回收率为90%~97%。采用标准曲线法对4种不同产地的西红花干燥柱头中硒进行了测定。该方法操作简单、快速,精密度好,准确性高,检出限较低,经济,便于推广应用。

  2. Speciation of the immediately mobilisable As(III), As(V), MMA and DMA in river sediments by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry following ultrasonic extraction

    Energy Technology Data Exchange (ETDEWEB)

    Huerga, A. [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Ciencias (Quimica), Universidad de Vigo, As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Lavilla, I. [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Ciencias (Quimica), Universidad de Vigo, As Lagoas-Marcosende s/n, 36200 Vigo (Spain); Bendicho, C. [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Ciencias (Quimica), Universidad de Vigo, As Lagoas-Marcosende s/n, 36200 Vigo (Spain)]. E-mail: bendicho@uvigo.es

    2005-04-04

    In this work, a fast method is developed for the speciation of As(III), As(V), MMA and DMA in the immediately mobilisable fraction of river sediments (i.e. water-soluble and phosphate-exchangeable) by high performance liquid chromatography-hydride generation-atomic fluorescence detection (HPLC-HG-AFD) after extraction using focused ultrasound. The influence of relevant parameters influencing an ion-pairing chromatographic separation following isocratic elution (i.e. amount of MeOH in the mobile phase, ion pair reagent concentration, pH, flow rate) was studied. Focused ultrasound transmitted from an ultrasonic probe provided the same extractable contents as conventional extraction with no changes in the species distribution. The effect of the drying step over extraction of As species was investigated. The following drying procedures were compared: freeze-, oven-, microwave- and air-drying. No influence of the drying operation on the water-extractable fraction was observed. However, freeze- and air-drying yielded significantly higher phosphate-extractable amounts of As(III) and As(V) as compared to oven and microwaves. Detection limits for the As species were in the range 1.3-4.1 ng/g for the water-soluble fraction and 1.6-4.8 ng/g for the phosphate buffer exchangeable fraction. The method was applied to the speciation of immediately mobilisable As(III), As(V), DMA and MMA in 11 sediment samples collected along the beds of the Louro River (southern Galicia, Spain)

  3. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solutions

    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, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solution to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Determination of Uranium 7 Specific Gravity by Pycnometry 15-20 Free Acid by Oxalate Complexation 21-27 Determination of Thorium 28 Determination of Chromium 29 Determination of Molybdenum 30 Halogens Separation by Steam Distillation 31-35 Fluoride by Specific Ion Electrode 36-42 Halogen Distillate Analysis: Chloride, Bromide, and Iodide by Amperometric Microtitrimetry 43 Determination of Chloride and Bromide 44 Determination of Sulfur by X-Ray Fluorescence 45 Sulfate Sulfur by (Photometric) Turbidimetry 46 Phosphorus by the Molybdenum Blue (Photometric) Method 54-61 Silicon by the Molybdenum Blue (Photometric) Method 62-69 Carbon by Persulfate Oxidation-Acid Titrimetry 70 Conversion to U3O8 71-74 Boron by ...

  4. Actinometry of Atomic Fluorine in a Capacitively Coupled Discharge with a mixture of SF6 and O2

    Science.gov (United States)

    Babu, Sharath; Swift, Paul; Daniels, Stephen; Turner, Miles

    2016-09-01

    Actinometry is a well-known technique for determining neutral species densities in reactive plasmas using optical emission spectroscopy. The basic idea is to compare the intensity of two emission lines, the first from a species of known density, and second from a species whose density is to be determined. Clearly, this approach succeeds only if the relationship between the relevant line intensities and the species densities is known. Actinometric measurement of atomic fluorine density is of special interest because alternative techniques, such as laser induced fluorescence, are impractically difficult for most purposes. In this paper we discuss actinometric measurement of fluorine densities in mixtures of SF6 and O2. In this system, the atomic neutral radical densities are a complex function of the gas mixture. Comparison of the actinometric data with mass spectrometric measurements shows that under many conditions they are proportional, so that ideal actinometric behaviour is observed. We show that this behaviour is predictable on the basis of a recently calculated excitation cross section for fluorine emission line. Hitherto, actinometry of fluorine has depended on difficult empirical calibration procedures. Work supported by the Irish Research Council and Intel Ireland Ltd.

  5. Mass spectrometric thermodynamic studies of oxide systems and materials

    Science.gov (United States)

    Stolyarova, V. L.

    2016-01-01

    Progress in methods of synthesis of advanced materials as well as utilization of such materials at high temperatures requires information on the vaporization processes and thermodynamic properties of oxide systems. The optimal experimental method for these purposes is high-temperature mass spectrometry. This review summarizes and classifies experimental results obtained in mass spectrometric studies of the high-temperature thermodynamic properties of oxide systems and materials carried out in the last two decades. Published data on the vaporization processes and thermodynamic properties of oxide materials for high-temperature technologies are discussed from the standpoint of acid-base concept and model approaches including statistical thermodynamic methods. The bibliography includes 248 references.

  6. E-2-benzylidenebenzocyclanones. II. IR and mass spectrometric investigations

    Science.gov (United States)

    Tarczay, Gy; Vékey, K.; Ludányi, K.; Perjési, P.; Sohár, P.

    2000-03-01

    A series of E-2-benzylideneindanones (a) -tetralones (b) and -benzosuberones (c) with OCH 3 ( 2- 4), NO 2 ( 5- 7) and F ( 8- 10) substituents in ortho, meta or para position was studied by IR and mass spectrometry. The most important IR bands were assigned and stated correlations between some frequencies and the stereostructure or conjugation feature of the molecules investigated. IR spectra were also analyzed in order to find frequencies characteristic of the size of the alkanone ring. The mass spectrometric investigation aimed at determining fragmentation pathways and finding correlations between them and the ring size of the alkanone ring or the position of the substituents.

  7. Rate of reaction of dimethylmercury with oxygen atoms in the gas phase

    DEFF Research Database (Denmark)

    Egsgaard, Helge

    1986-01-01

    The rate constant for the reaction of atomic oxygen (O(3P)) with dimethylmercury has been measured at room temperature at a pressure of about 1 Torr using a fast flow system with electron paramagnetic resonance and mass spectrometric detection. Some reaction products were identified. The rate...

  8. 微波消解-氢化物发生-原子荧光光谱法同时测定鱼罐头中砷和汞%Simultaneous determination of arsenic and mercury in canned fish by microwave digestion - hydride generation - atomic fluorescence spectrometric

    Institute of Scientific and Technical Information of China (English)

    唐开红

    2012-01-01

    目的 建立一种同时测定鱼罐头中砷和汞含量的方法.方法 微波消解样品后,用氢化物发生-原子荧光光谱法测定砷和汞含量.结果 砷、汞测定液的检出限分别为0.049μg/L、0.017μg/L,回收率分别为98.2%~106.2%、98.4%~104.2%;相对标准偏差分别为1.7%~2.8%、1.8%~3.1%.结论 本实验方法简单快速,重现性好,准确度高,线性范围宽,适合测定鱼罐头中砷和汞的含量.

  9. Synchronous determination of arsenic and mercury in organic-inorganic compound fertilizer by microwave digestion——atomic fluorescence spectrometric method (AFS)%微波消解——原子荧光光谱法同时测定有机-无机复混肥料中砷和汞的含量

    Institute of Scientific and Technical Information of China (English)

    宋吉利; 于春霞; 于作文; 张书文

    2006-01-01

    采用微波消解样品预处理技术和原子荧光光谱法同时测定有机-无机复混肥料中的砷和汞,确定微波消解样品的条件,优化仪器的最佳工作参数.砷和汞的含量分别在0~20μg/L和0~10 μg/L范围内有良好线性关系,砷和汞的回收率分别在99.1%~102.0%和98.1%~101.5%,砷和汞的检出限(3σ)分别为0.20 μg/L和0.070μg/L.实验表明,该方法具有操作简单、快速、灵敏度高等优点,可适用于有机-无机复混肥料中砷和汞的同时测定.

  10. Nondestructive characterization of municipal-solid-waste-contaminated surface soil by energy-dispersive X-ray fluorescence and low-Z (atomic number) particle electron probe X-ray microanalysis.

    Science.gov (United States)

    Gupta, Dhrubajyoti; Ghosh, Rita; Mitra, Ajoy K; Roy, Subinit; Sarkar, Manoranjan; Chowdhury, Subhajit; Bhowmik, Asit; Mukhopadhyay, Ujjal; Maskey, Shila; Ro, Chul-Un

    2011-11-01

    The long-term environmental impact of municipal solid waste (MSW) landfilling is still under investigation due to the lack of detailed characterization studies. A MSW landfill site, popularly known as Dhapa, in the eastern fringe of the metropolis of Kolkata, India, is the subject of present study. A vast area of Dhapa, adjoining the current core MSW dump site and evolving from the raw MSW dumping in the past, is presently used for the cultivation of vegetables. The inorganic chemical characteristics of the MSW-contaminated Dhapa surface soil (covering a 2-km stretch of the area) along with a natural composite (geogenic) soil sample (from a small countryside farm), for comparison, were investigated using two complementary nondestructive analytical techniques, energy-dispersive X-ray fluorescence (EDXRF) for bulk analysis and low-Z (atomic number) particle electron probe X-ray microanalysis (low-Z particle EPMA) for single-particle analysis. The bulk concentrations of K, Rb, and Zr remain almost unchanged in all the soil samples. The Dhapa soil is found to be polluted with heavy metals such as Cu, Zn, and Pb (highly elevated) and Ti, Cr, Mn, Fe, Ni, and Sr (moderately elevated), compared to the natural countryside soil. These high bulk concentration levels of heavy metals were compared with the Ecological Soil Screening Levels for these elements (U.S. Environment Protection Agency) to assess the potential risk on the immediate biotic environment. Low-Z particle EPMA results showed that the aluminosilicate-containing particles were the most abundant, followed by SiO2, CaCO3-containing, and carbonaceous particles in the Dhapa samples, whereas in the countryside sample only aluminosilicate-containing and SiO2 particles were observed. The mineral particles encountered in the countryside sample are solely of geogenic origin, whereas those from the Dhapa samples seem to have evolved from a mixture of raw dumped MSW, urban dust, and other contributing factors such as wind

  11. Determination of Arsenic and Antimony in Leather by Atomic Fluorescence Spectrometry with Microwave Digestion%微波消解—原子荧光光谱法同时测定皮革中的砷和锑

    Institute of Scientific and Technical Information of China (English)

    吕小园; 陈新焕; 肖家勇; 刘正华; 陈练; 杨万彪; 黄红; 张志荣

    2012-01-01

    建立了皮革及其制品中砷和锑的微波消解-原子荧光光谱测定方法,方法准确、灵敏,快速.在优化的试验条件下,砷浓度在0.5~150 ng/mL范围内成线性关系,相关系数r=0.9995,检出限为0.22 ng/mL,回收率为99.4%~104.2%:锑浓度在0.5~ 120 ng/mL范围内成线性关系,相关系数r=0.9998,检出限为0.16 ng/mL,回收率为101.1%~106.7%.相对标准偏差(n=5)均小于5%.方法应用于皮革及其制品中砷和锑的测定,结果满意.%An accurate, sensitive and quick method for determination of arsenic and antimony in leather by atomic fluorescence spectrometry with microwave digestion was developed in this paper. Under the optimized condition, the result of arsenic showed that the linear range was 0.5 - 150 ng/mL(r =0. 9995), the limit of detection was 0. 22 ng/mL, and the average recoveries in leather ranged form 99. 4% to 104. 2% . The linear range of antimony was 0. 5 ~ 120 ng/mL( r = 0.9998) , the limit of detection was 0. 16 ng/mL, the average recoveries ranged form 101. 1% tol06.7%. TheRSD(n=5) were all lower than 5%. It has been applied to routine determination of arsenic and antimony in leather with satisfactory results.

  12. Determination of Arsenic and Mercury in Soil by Atomic Fluorescence Spectrometry with Aquafortis Bath Digestion%王水消解-原子荧光光谱法测定土中砷和汞

    Institute of Scientific and Technical Information of China (English)

    杜英秋

    2013-01-01

    To explore new methods of determinating arsenic and mercury in soil ,through atomic fluorescence spectrometry with aquafortis digestion ,arsenic and mercury in soil samples were determinated .The results showed that good linear relationship when concentrations of arsenic was 0~100 ng·mL-1 and mercury was 0~2 .0 ng·mL-1 ,the correlation coefficient were 0 .999 9 and 0 .999 3 respectively ,the detection limits were 0 .260 and 0 .022 ng·mL-1 ,the method was used for the determination of arsenic and mercury in different soil standard materials ,results were in the standard value range ,RSD was 1 .3% ~3 .5% ,that indicatd that the method had wide linear range ,good stability ,high sensitivity ,high accuracy and it could be widely used for the determina-tion of arsenic and mercury in bulk soil samples .%为探讨检测土壤中砷和汞的新方法,采用王水-水体系进行消解,应用原子荧光光谱法对土壤样品中的砷和汞进行测定。结果表明:当砷的质量浓度处于0~100.0 ng·mL-1,汞的质量浓度处于0~2.0 ng·mL-1时,浓度与荧光强度均能呈良好的线性关系,相关系数分别为0.9999和0.9993,方法的检出限分别为0.260和0.022 ng·mL-1,将该方法用于不同土壤标准物质的测定,测定结果均在标准值允许范围内,RSD处于1.3%~3.5%,说明该方法线性范围宽,稳定性好,灵敏度高,准确度高,可广泛用于批量土样中砷和汞的测定。

  13. Simultaneous determination of arsenic and antimony in water by hydride generation-atomic fluorescence spectrometry%同时测定水中砷和锑的氢化物发生-原子荧光光谱法

    Institute of Scientific and Technical Information of China (English)

    宋岳; 周虹

    2012-01-01

    目的 建立双道原子荧光光度计同时测定饮用水中砷和锑的方法,以提高工作效率.方法 选择最佳的仪器条件,进行样品处理方法及酸度、硼氢化钾浓度、检出限、线性范围、精密度、加标回收率等研究.结果 该方法线性关系:砷为0 ~ 80 μg/L,锑为O~40μg/L.检出限:砷为0.087 μg/L,锑为0.19μg/L.相对标准偏差:砷为1.93% ~ 2.55%;锑为1.97% ~3.02%.平均加标回收率:砷为95.7%;锑为96.5%.结论 该方法操作简便,灵敏度高,快速,便于推广,适用于水中砷和锑的同时测定.%[ Objective]To establish the method for simultaneous determination of arsenic and antimony in drinking water by double channel atomic fluorescence spectrometer, improve work efficiency. [Methods]Choosing optimal instrument condition, the sample treatment method, acidity, concentration of potassium borohydride, detection limit, linear range, precision and the recovery of standard addition were studied. [Results]The linear relationship of arsenic and antimony was 0-80μg/L and 0-40 μg/L respectively. The detection limit of arsenic and antimony was 0.087 μg/L and 0.19 μg/L respectively. The relative standard deviation of arsenic and antimony was 1.93% -2. 55% and 1. 97% -3. 02% respectively. The average recovery of standard addition of arsenic and antimony was 95.7% and 96.5% respectively. [ Conclusion] This method has the advantages of simple operation and high sensitivity , it is rapid and easy to spread, which is suitable for simultaneous determination of arsenic and antimony in water.

  14. Determination of arsenic in urine by wet digestion-hydride generation atomic fluorescence spectrometry%湿法消化-氢化物原子荧光法测定尿中砷

    Institute of Scientific and Technical Information of China (English)

    张克梅; 王文静

    2011-01-01

    Objective: To establish an accurate and simple determination of universal detection of arsenic in urine. Methods:Mixed acid sample digestion in the electric panel heating with thiourea, ascorbic acid to pentavalent arsenic to trivalent arsenic pre -reduction, and then potassium borohydride as reducing agent, to 5% HNO3 as the medium, with the AFS-230E direct determination of atomic fluorescence spectrometer. Results: The optimal experimental conditions, good linearity was presented within the arsenic concentration range of 0.0 μg/L ~ 20.0 μg/L; and the correlation coefficient was 0.9999, the lowest detection limit of the method was 0. 164 μg/L, relative standard deviation (RSD) was 0.4% ~ 1.2%, the recovery was 98.6% ~103.5%. Conclusion: The method is simple, precise, which high recovery rate, which is to determine a reliable method ofurinary arsenic.%目的:建立一种准确简单易于普及的测定尿中砷的检测方法.方法:样品用混合酸在电热板上加热消解后,用硫脉抗坏血酸将五价砷预还原为三价砷,再用硼氢化钾作还原剂,以5% HNO3为介质,用AF5-230E原子荧光光度计直接测定.结果:在最佳实验条件下,砷的浓度在0.0 μg/L~20.0 μg/L之间线性关系良好,相关系数r= 0.9999,方法的最低检出限为0.164 μg/L,RSD为0.4%~1.2%,加标回收率为98.6%~103.5%.结论:该方法操作简单,精密度好,回收率高,是测定尿砷含量的可靠方法.

  15. Mass spectrometric study of the thermochemistry of gaseous EuTiO3 and TiO2

    Science.gov (United States)

    Balducci, G.; Gigli, G.; Guido, M.

    1985-08-01

    The gaseous molecule EuTiO3 has been investigated in a high temperature mass spectrometric study of vapors over the europium-titanium-oxygen system. From the enthalpy of reaction: EuTiO3(g)=EuO(g)+TiO2(g) and proper ancillary data, the atomization energy of this molecule has been determined. In addition, from the study of the gaseous exchange reaction: TiO2(g)+Eu(g)=TiO(g)+EuO(g) the dissociation energy of TiO2(g) has been derived and compared with previous results. The dissociation energies proposed are: D○0,at(EuTiO3) =2278±28 kJ mol-1 and D○0,at(TiO2) =1260±12 kJ mol-1.

  16. [Application of PCA to diesel engine oil spectrometric analysis].

    Science.gov (United States)

    Liu, Tao; Tian, Hong-Xiang; Guo, Wen-Yong

    2010-03-01

    In order to study wear characteristics of a 6-cylinder diesel engine, six different working statuses were arranged by altering the clearance between cylinder and piston. Sixty-nine oil samples were taken from engine at different loads under 6 working statuses and analyzed by Spectroil M Instrument made in US. Principal component analysis (PCA) was applied to analyzing spectrometric data of sixty-nine oil samples and clustering those data according to elements and oil samples separately based on the weighted coefficient and principal component scores. All 21 elements were used in element clustering and only 6 wear-related elements, namely iron, chromium, aluminum, copper, plumbum and silicon, were used in sample clustering. It is shown that PCA effectively clustered oil spectrometric data into three different principal components according to elements. The projection of two different principal components exhibited five types of elements combinations, namely wear elements (Fe, Cr, Cu, Al and Pb), high concentration additives elements (Na, Zn, P, Ca and Mg), low concentration additives elements (Ba and B), base constituent of lubricating oils (C and H) and interferential elements (Ni, Ti, Mo, V, Ag and Sn). Furthermore, PCA clearly clustered oil samples according to different clearance between cylinder and piston in the diesel engine. The study suggests that analyzing oil spectrographic data by PCA could find the sources of different elements, monitor engine conditions and diagnose wear faults.

  17. Targeted quantitative mass spectrometric immunoassay for human protein variants

    Directory of Open Access Journals (Sweden)

    Nedelkov Dobrin

    2011-04-01

    Full Text Available Abstract Background Post-translational modifications and genetic variations give rise to protein variants that significantly increase the complexity of the human proteome. Modified proteins also play an important role in biological processes. While sandwich immunoassays are routinely used to determine protein concentrations, they are oblivious to protein variants that may serve as biomarkers with better sensitivity and specificity than their wild-type proteins. Mass spectrometry, coupled to immunoaffinity separations, can provide an efficient mean for simultaneous detection and quantification of protein variants. Results Presented here is a mass spectrometric immunoassay method for targeted quantitative proteomics analysis of protein modifications. Cystatin C, a cysteine proteinase inhibitor and a potential marker for several pathological processes, was used as a target analyte. An internal reference standard was incorporated into the assay, serving as a normalization point for cystatin C quantification. The precision, linearity, and recovery characteristics of the assay were established. The new assay was also benchmarked against existing cystatin C ELISA. In application, the assay was utilized to determine the individual concentration of several cystatin C variants across a cohort of samples, demonstrating the ability to fully quantify individual forms of post-translationally modified proteins. Conclusions The mass spectrometric immunoassays can find use in quantifying specific protein modifications, either as a part of a specific protein biomarker discovery/rediscovery effort to delineate the role of these variants in the onset of the disease, progression, and response to therapy, or in a more systematic study to delineate and understand human protein diversity.

  18. Detection of formestane abuse by mass spectrometric techniques.

    Science.gov (United States)

    de la Torre, Xavier; Colamonici, Cristiana; Curcio, Davide; Jardines, Daniel; Molaioni, Francesco; Parr, Maria Kristina; Botrè, Francesco

    2014-01-01

    Formestane (4-hydroxy-androstenedione) is an aromatase inhibitor prohibited in sports and included, since 2004, in the list of prohibited substances updated yearly by the World Anti-Doping Agency (WADA). Since the endogenous production of formestane has been described, it is mandatory for the anti-doping laboratories to use isotope ratio mass spectrometry (IRMS) to establish the exogenous origin before issuing an adverse analytical finding. The described IRMS methods for formestane detection are time-consuming, requiring usually two consecutive liquid chromatographic sample purifications in order to have final extracts of adequate purity before the mass spectrometric analysis. After establishing a procedure for the determination of the origin of formestane by IRMS without the need of derivatization, and integrated in the overall analytical strategy of the laboratory for pseudo-endogenous steroids, a mass spectrometric analysis by gas chromatography-mass spectrometry (GC-MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS) of formestane metabolites was carried out in order to investigate whether other biomarkers of formestane abuse could be integrated in order to avoid time-consuming and expensive IRMS confirmations for formestane. From the metabolic studies performed, the inclusion of 3β,4α-dihydroxy-5α-androstan-17-one (4α-hydroxy-epiandosterone) in the routine GC-MS procedures has demonstrated to be diagnostic in order to reduce the number of unnecessary confirmations of the endogenous origin of formestane.

  19. Advanced ultrasound-assisted sample pre-treatment for trace elemental analysis by atomic spectrometric techniques

    OpenAIRE

    2012-01-01

    Esta Tesis Doctoral se centra en la preparación de muestra, que es una etapa esencial en el proceso analítico. La simplificación, automatización y miniaturización de esta etapa son algunas de las tendencias más recientes en la Química Analítica. Además, la implementación de protocolos limpios Green Chemistry son altamente demandados. En este aspecto, los ultrasonidos proporcionan varias ventajas cuando se aplica a la etapa de preparación de muestra, ya que se trata de una energía limpia y efi...

  20. Atom chips

    CERN Document Server

    Reichel, Jakob

    2010-01-01

    This book provides a stimulating and multifaceted picture of a rapidly developing field. The first part reviews fundamentals of atom chip research in tutorial style, while subsequent parts focus on the topics of atom-surface interaction, coherence on atom chips, and possible future directions of atom chip research. The articles are written by leading researchers in the field in their characteristic and individual styles.

  1. Atomic energy

    CERN Multimedia

    1996-01-01

    Interviews following the 1991 co-operation Agreement between the Department of Atomic Energy (DAE) of the Government of India and the European Organization for Nuclear Research (CERN) concerning the participation in the Large Hadron Collider Project (LHC) . With Chidambaram, R, Chairman, Atomic Energy Commission and Secretary, Department of Atomic Energy, Department of Atomic Energy (DAE) of the Government of India and Professor Llewellyn-Smith, Christopher H, Director-General, CERN.

  2. Ultraviolet irradiation-induced substitution of fluorine with hydroxyl radical for mass spectrometric analysis of perfluorooctane sulfonyl fluoride

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Peng; Tang, Xuemei; Huang, Lulu; Kang, Jie; Zhong, Hongying, E-mail: hyzhong@mail.ccnu.edu.cn

    2016-01-28

    A rapid and solvent free substitution reaction of a fluorine atom in perfluorooctane sulfonyl fluoride (PFOSF) with a hydroxyl radical is reported. Under irradiation of ultraviolet laser on semiconductor nanoparticles or metal surfaces, hydroxyl radicals can be generated through hole oxidization. Among all fluorine atoms of PFOSF, highly active hydroxyl radicals specifically substitute the fluorine of sulfonyl fluoride functional group. Resultant perfluorooctane sulfonic acid is further ionized through capture of photo-generated electrons that switch the neutral molecules to negatively charged odd electron hypervalent ions. The unpaired electron subsequently initiates α O–H bond cleavage and produces perfluorooctane sulfonate negative ions. Hydroxyl radical substitution and molecular dissociation of PFOSF have been confirmed by masses with high accuracy and resolution. It has been applied to direct mass spectrometric imaging of PFOSF adsorbed on surfaces of plant leaves. - Highlights: • Ultraviolet irradiation on semiconductor nanoparticles produces electron–hole pairs. • Hole oxidization results in the formation of hydroxyl radicals. • Fluorine atoms of PFOSF can be specifically substituted with hydroxyl radicals. • Capture of photoelectrons causes dissociation and fragmentation. • Fragments are detected in negative ion mode.

  3. Fluorescent microspheres

    Science.gov (United States)

    Rembaum, A.

    1978-01-01

    Latex particles with attached antibodies have potential biochemical and environmental applications. Human red blood cells and lymphocytes have been labeled with fluorescent microspheres by either direct or indirect immunological technique. Immunolatex spheres can also be used for detecting and localizing specific cell surface receptors. Hormones and toxins may also be bondable.

  4. Atomic polarizabilities

    Energy Technology Data Exchange (ETDEWEB)

    Safronova, M. S. [Department of Physics and Astronomy, University of Delaware, Newark, DE 19716 (United States); Mitroy, J. [School of Engineering, Charles Darwin University, Darwin NT 0909 (Australia); Clark, Charles W. [Joint Quantum Institute, National Institute of Standards and Technology and the University of Maryland, Gaithersburg, Maryland 20899-8410 (United States); Kozlov, M. G. [Petersburg Nuclear Physics Institute, Gatchina 188300 (Russian Federation)

    2015-01-22

    The atomic dipole polarizability governs the first-order response of an atom to an applied electric field. Atomic polarization phenomena impinge upon a number of areas and processes in physics and have been the subject of considerable interest and heightened importance in recent years. In this paper, we will summarize some of the recent applications of atomic polarizability studies. A summary of results for polarizabilities of noble gases, monovalent, and divalent atoms is given. The development of the CI+all-order method that combines configuration interaction and linearized coupled-cluster approaches is discussed.

  5. 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.

  6. 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.

  7. 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

  8. 氢化物原子荧光光谱法同时测定生活饮用水中砷和硒%Simulatneous Determination of Arsenic and selenium in Drinking Water Samples by Hydride Generation Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    张祥楼

    2014-01-01

    建立了氢化物发生原子荧光光谱法同时测定生活饮用水中砷和硒的方法.测试结果表明砷和硒在质量浓度分别为0.00μg/L~10.00μg/L和0.00μg/L~40.00μg/L范围内呈线性关系,相关系数分别为(砷r=0.9998,硒r=0.9997)。仪器检出限为砷:0.03μg/L硒:0.05μg/L。本方法检出限砷为0.075μg/L;硒为0.125μg/L。水质样品中砷的回收率为92.6%~96.5%,精密度为0.8%~1.4%;硒的回收率为91.2%~97.4%,精密度为1.0%~1.6%。应用本方法测定生活饮用水中的砷和硒方法简便、快速,结果准确可靠,较好地提高了工作效率。%A method for simulatneous determination of Arsenic and selenium in drinking water samples by hydride generation atomic fluorescence spectrometry.As a matter of fact ,the linear range of Arsenic was 0.00μg/L~10.00μg/L and the related coefficient was 0.9998;While the linear range of Selenium was 0.00μg/L~40.00μg/L and the related coefficient was0.9997. Instrument detection limit was 0.03μg/L(arsenic)and 0.05μg/L(selenium).Detection limits of the method was 0.075μg/L (arsenic)and 0.125μg/L(selenium). The rate of arsenic recovery was 92.6%~96.5%and the precision in the drinking water was in the range of 0.8%~1.4%.while the rate of selenium recovery was 92.6%~96.5%and the precision in the drinking water was in the range of 1.0%~1.6%.The experimental results shows that the method is applicable .

  9. 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.

  10. Fluorescence Microscopy of Nanoscale Silver Oxide Thin Films

    Institute of Scientific and Technical Information of China (English)

    PAN Xin-Yu; JIANG Hong-Bing; LIU Chun-Ling; GONG Qi-Huang; ZHANG Xi-Yao; ZHANG Qi-Feng; XU Bei-Xue; WU Jin-Lei

    2003-01-01

    The experimental conditions for photoactivated intermittent fluorescence from nanoscale silver oxide were studied with fluorescence microscopy. Strong fluorescence was observed from the Ag?O particles with size of 10-20nm excited with both blue and green light. We observed the saturation of photoexcitation with blue light and explained the experimental results using the model of agglomeration of silver atoms to form small clusters and the fluorescence of Ag2 and Ags clusters.

  11. 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

  12. Molecular-sized fluorescent nanodiamonds

    Science.gov (United States)

    Vlasov, Igor I.; Shiryaev, Andrey A.; Rendler, Torsten; Steinert, Steffen; Lee, Sang-Yun; Antonov, Denis; Vörös, Márton; Jelezko, Fedor; Fisenko, Anatolii V.; Semjonova, Lubov F.; Biskupek, Johannes; Kaiser, Ute; Lebedev, Oleg I.; Sildos, Ilmo; Hemmer, Philip. R.; Konov, Vitaly I.; Gali, Adam; Wrachtrup, Jörg

    2014-01-01

    Doping of carbon nanoparticles with impurity atoms is central to their application. However, doping has proven elusive for very small carbon nanoparticles because of their limited availability and a lack of fundamental understanding of impurity stability in such nanostructures. Here, we show that isolated diamond nanoparticles as small as 1.6 nm, comprising only ~400 carbon atoms, are capable of housing stable photoluminescent colour centres, namely the silicon vacancy (SiV). Surprisingly, fluorescence from SiVs is stable over time, and few or only single colour centres are found per nanocrystal. We also observe size-dependent SiV emission supported by quantum-chemical simulation of SiV energy levels in small nanodiamonds. Our work opens the way to investigating the physics and chemistry of molecular-sized cubic carbon clusters and promises the application of ultrasmall non-perturbative fluorescent nanoparticles as markers in microscopy and sensing.

  13. 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.

  14. Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

    Science.gov (United States)

    Campos, Reinaldo C.; Gonçalves, Rodrigo A.; Brandão, Geisamanda P.; Azevedo, Marlo S.; Oliveira, Fabiana; Wasserman, Julio

    2009-06-01

    The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C 18 column was used as stationary phase, and post column treatment was performed by UV irradiation (60 °C, 13 W). The eluate was then merged with 3 mol L - 1 HCl, reduction was performed by a NaBH 4 solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 µg L - 1 were obtained for ionic (Hg 2+) and HgCH 3+, for an injection volume of 200 µL. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sediments.

  15. Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

    Energy Technology Data Exchange (ETDEWEB)

    Campos, Reinaldo C. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil)], E-mail: rccampos@puc-rio.br; Goncalves, Rodrigo A.; Brandao, Geisamanda P.; Azevedo, Marlo S. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil); Oliveira, Fabiana; Wasserman, Julio [Institut of Geosciences, Fluminense Federal University, Av. Gal. Milton Tavares de Souza, s/n, 24.210-340, Niteroi, Rio de Janeiro (Brazil)

    2009-06-15

    The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C{sub 18} column was used as stationary phase, and post column treatment was performed by UV irradiation (60 deg. C, 13 W). The eluate was then merged with 3 mol L{sup -1} HCl, reduction was performed by a NaBH{sub 4} solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 {mu}g L{sup -1} were obtained for ionic (Hg{sup 2+}) and HgCH{sub 3}{sup +}, for an injection volume of 200 {mu}L. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sedi0011men.

  16. Study on determination of lead in aluminium polychlorid by continuous flow-hydride generation atomic fluorescence spectrometry%连续流动-氢化物发生原子荧光光谱法测定聚合氯化铝中铅

    Institute of Scientific and Technical Information of China (English)

    龚胜芳; 高树林; 李志华; 王红柳

    2014-01-01

    采用连续流动-氢化物发生原子荧光光谱法(CF-HGAFS)测定聚合氯化铝中的铅,优化了实验条件,在最佳实验条件下,铅的荧光强度在0~25μg /L范围内与浓度呈良好的线性关系,方法检出限为0.043μg/L ,方法回收率在95.3%~105.6%之间,本法操作简便、快捷,而且具有很好的准确性和精密度,应用前景良好。%A method for the determination of lead in aluminium polychlorid by continuous flow-hydride generation atomic fluorescence spectrometry was established .The effect of experimental conditions on the atomic fluorescence intensity were investigated and optimized .In this condition ,the calibration curve was linear up to 25μg/L ,the detection limit was 0 .043μg/L ,and the recovery was in range of 95 .3%-105.6% . The method is not only simple and rapid but also precise and accurate ,and shows good application pros-pects .

  17. The Mechanism of 2-Furaldehyde Formation from d-Xylose Dehydration in the Gas Phase. A Tandem Mass Spectrometric Study

    Science.gov (United States)

    Ricci, Andreina; Piccolella, Simona; Pepi, Federico; Garzoli, Stefania; Giacomello, Pierluigi

    2013-07-01

    The mechanism of reactions occurring in solution can be investigated also in the gas phase by suited mass spectrometric techniques, which allow to highlight fundamental mechanistic features independent of the influence of the medium and to clarifying controversial hypotheses proposed in solution studies. In this work, we report a gas-phase study performed by electrospray triple stage quadrupole mass spectrometry (ESI-TSQ/MS) on the dehydration of d-xylose, leading mainly to the formation of 2-furaldehyde (2-FA). It is generally known in carbohydrate chemistry that the thermal acid catalyzed dehydration of pentoses leads to the formation of 2-FA, but several aspects on the solution-phase mechanism are controversial. Here, gaseous reactant ions corresponding to protonated xylose molecules obtained from ESI of a solution containing d-xylose and ammonium acetate as protonating reagent were allowed to undergo collisionally activated decomposition (CAD) into the triple stage quadrupole analyzer. The product ion mass spectra of protonated xylose are characterized by the presence of ionic intermediates arising from xylose dehydration, which were structurally characterized by their fragmentation patterns. As expected, the xylose triple dehydration leads to the formation of the ion at m/z 97, corresponding to protonated 2-FA. On the basis of mass spectrometric evidences, we demonstrated that in the gas phase, the formation of 2-FA involves protonation at the OH group bound to the C1 atom of the sugar, the first ionic intermediate being characterized by a cyclic structure. Finally, energy resolved product ion mass spectra allowed to obtain information on the energetic features of the d-xylose→2-FA conversion.

  18. Atomic physics

    CERN Document Server

    Born, Max

    1989-01-01

    The Nobel Laureate's brilliant exposition of the kinetic theory of gases, elementary particles, the nuclear atom, wave-corpuscles, atomic structure and spectral lines, electron spin and Pauli's principle, quantum statistics, molecular structure and nuclear physics. Over 40 appendices, a bibliography, numerous figures and graphs.

  19. In situ direct sampling mass spectrometric study on formation of polycyclic aromatic hydrocarbons in toluene pyrolysis.

    Science.gov (United States)

    Shukla, Bikau; Susa, Akio; Miyoshi, Akira; Koshi, Mitsuo

    2007-08-30

    The gas-phase reaction products of toluene pyrolysis with and without acetylene addition produced in a flow tube reactor at pressures of 8.15-15.11 Torr and temperatures of 1136-1507 K with constant residence time (0.56 s) have been detected in an in situ direct sampling mass spectrometric study by using a vacuum ultraviolet single-photon ionization time-of-flight mass spectrometry technique. Those products range from methyl radical to large polycyclic aromatic hydrocarbons (PAHs) of mass 522 amu (C(42)H(18)) including smaller species, radicals, polyynes, and PAHs, together with ethynyl, methyl, and phenyl PAHs. On the basis of observed mass spectra, the chemical kinetic mechanisms of the formation of products are discussed. Especially, acetylene is mixed with toluene to understand the effect of the hydrogen abstraction and acetylene addition (HACA) mechanism on the formation pathways of products in toluene pyrolysis. The most prominent outputs of this work are the direct detection of large PAHs and new reaction pathways for the formation of PAHs with the major role of cyclopenta-fused radicals. The basis of this new reaction route is the appearance of different sequences of mass spectra that well explain the major role of aromatic radicals mainly cyclopenta fused radicals of PAHs resulting from their corresponding methyl PAHs, with active participation of c-C(5)H(5), C(6)H(5), C(6)H(5)CH(2) ,and C(9)H(7) in the formation of large PAHs. The role of the HACA only seemed important for the formation of stable condensed PAHs from unstable primary PAHs with zigzag structure (having triple fusing sites) in one step by ring growth with two carbon atoms.

  20. Status of mass spectrometric radiocarbon detection at ETHZ

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-10-15

    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 {sup 14}C 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{sup +} 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.

  1. 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

    2012-08-07

    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.

  2. 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.

  3. Gamma Spectrometric Analysis of Iron Ore Samples of Arak, Iran

    Directory of Open Access Journals (Sweden)

    Reza Pourimani

    2016-09-01

    Full Text Available Introduction Iron ore is one of the most important natural raw materials that is widely used for manufacturing iron and steel. This type of ore contains various amounts of radionuclides; thus, exposing workers handling their extraction, transportation, and processing to radiation. Materials and Methods In this study, 12 ore samples (each mass weighing about 2 kg were collected from the iron ore mining areas of Arak region, Iran. The specific activities of 226Ra, 232Th, and 40K were determined usinggamma-ray spectrometry method employing high-purity germanium (HPGe detector. Results The specific activities of 226Ra, 232Th, and 40K in samples were 9.39-271.70 Bq/kg, -3 Sv/y suggested in International Commission of Radiological Protection (ICRP Publication 82. Conclusion The gamma ray spectrometric analysis showed that the specific activities of natural radionuclides in samples, except for limonite ore, were within the worldwide range. The effective dose received by workers was much lower than the maximum acceptable value (1000 μSv/y; therefore, the level of radiations in this mine had no adverse consequences for public health.

  4. 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.

  5. Fluorescence-Based Sensors

    Science.gov (United States)

    Orellana, Guillermo

    The natural luminescent phenomena (from the Latin words "lumen" and "essentia", i.e., "made of light") such as northern lights (aurora borealis), marine brightness, glow-worms, shining putrid fish scales, "bluish"- appearing water when contained in certain wooden cups (quinine fluorescence), some stones heated at high temperatures with reducing agents (BaS phosphorescence), or light emitted while crushing sugar (triboluminescence) already fascinated our ancestors. Nowadays we understand that ultraviolet and visible emission of light originates from a competitive deactivation pathway of the lowest electronic excited state of atoms and molecules that produces the so called luminescence (the sub-terms fluorescence and phosphorescence just designate whether the return of the excited to the ground state is an "allowed" or "forbidden" process, namely it is fast or slow, the loosely-defined border between them being a 1-μs-1 rate constant). Actually, luminescence is the only method to generate light in the known Universe regardless it is powered by the nuclear reactions in the stars, the ohmical heating in bulbs, an electric discharge, the absorption of light or a (bio)chemical reaction (chemiluminescence).

  6. Peptide-stabilized, fluorescent silver nanoclusters

    DEFF Research Database (Denmark)

    Gregersen, Simon; Vosch, Tom André Jos; Jensen, Knud Jørgen

    2016-01-01

    . Herein, we demonstrate how solid-phase methods can increase throughput dramatically in peptide ligand screening and in initial evaluation of fluorescence intensity and chemical stability of peptide-stabilized AgNCs (P-AgNCs). 9-Fluorenylmethyloxycarbonyl (Fmoc) solid-phase peptide synthesis......Few-atom silver nanoclusters (AgNCs) can exhibit strong fluorescence; however, they require ligands to prevent aggregation into larger nanoparticles. Fluorescent AgNCs in biopolymer scaffolds have so far mainly been synthesized in solution, and peptides have only found limited use compared to DNA...

  7. The spectroscopy in the atomic vapour

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jai Hyung; Chang, Joon Sung; Jhe, Won Ho [Seoul National University, Seoul (Korea)

    1998-04-01

    As spectroscopies in the atomic vapor, we perform experiments on fluorescence in dense atomic vapor, single color two-photon resonant three photon ionization, production of high temperature oven and its spectroscopic application, atomic trap and cold atomic beam. We observe lengthening of lifetime as atomic density increase and compare this result with Holstein equation. Dependence on pressure an d polarization reveals the result is due to collisions between Yb atom and Ar buffer gas. At high atomic density, self-focusing and conical emission are observed. In two-photon resonant three photon ionization scheme, ionization rate is dependent on polarization. From selection rule, we determined the energy level. At higher energy, asymmetry and broadening of ionization linewidth due to AC Stark effect are observed. As the result of numerical simulation of time evolution in the two-photon transition, distortion of time evolution of density is obtained. For spectroscopy of high-melting-point elements, we design and produce high temperature oven. We observe absorption spectra of high-melting-point elements, Er and Sm. As high temperature nonlinear spectroscopies, we perform conical emission and self-diffraction in Sm vapor. We produce magneto-optical trap system and measure fluorescence from trapped atoms and temperature. By trapping Rb isotopes simultaneously, we perform collision experiment at low temperature. Using hollow mirror system, we trap atoms and produce cold atomic beam. (author). 160 refs., 66 figs., 5 tabs.

  8. 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.

  9. Oxidative Ionization Under Certain Negative-Ion Mass Spectrometric Conditions

    Science.gov (United States)

    Hassan, Isra; Pavlov, Julius; Errabelli, Ramu; Attygalle, Athula B.

    2017-02-01

    1,4-Hydroquinone and several other phenolic compounds generate (M - 2) -• radical-anions, rather than deprotonated molecules, under certain negative-ion mass spectrometric conditions. In fact, spectra generated under helium-plasma ionization (HePI) conditions from 1,4-hydroquinone and 1,4-benzoquinone (by electron capture) were practically indistinguishable. Because this process involves a net loss of H• and H+, it can be termed oxidative ionization. The superoxide radical-anion (O2 -•), known to be present in many atmospheric-pressure plasma ion sources operated in the negative mode, plays a critical role in the oxidative ionization process. The presence of a small peak at m/z 142 in the spectrum of 1,4-hydroquinone, but not in that of 1,4-benzoquinone, indicated that the initial step in the oxidative ionization process is the formation of an O2 -• adduct. On the other hand, under bona fide electrospray ionization (ESI) conditions, 1,4-hydroquinone generates predominantly an (M - 1) - ion. It is known that at sufficiently high capillary voltages, corona discharges begin to occur even in an ESI source. At lower ESI capillary voltages, deprotonation predominates; as the capillary voltage is raised, the abundance of O2 -• present in the plasma increases, and the source in turn increasingly behaves as a composite ESI/APCI source. While maintaining post-ionization ion activation to a minimum (to prevent fragmentation), and monitoring the relative intensities of the m/z 109 (due to deprotonation) and 108 (oxidative ionization) peaks recorded from 1,4-hydroquinone, a semiquantitative estimation of the APCI contribution to the overall ion-generation process can be obtained.

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

    Energy Technology Data Exchange (ETDEWEB)

    Bugalho, R; Carrico, B; Ferreira, C S; Frade, M; Ferreira, M; Moura, R; Ortigao, C; Pinheiro, J F; Rodrigues, P; Rolo, I; Silva, J C; Trindade, A; Varela, J [Laboratorio de Instrumentacao e Fisica Experimental de Particulas (LIP), Av. Elias Garcia 14-1, 1000-149 Lisboa (Portugal)], E-mail: frade@lip.pt

    2009-10-15

    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 Portugues 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 x 2 x 20 mm{sup 3} 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 C{sub DOI}{sup -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.

  11. 高效液相色谱氢化物发生原子荧光光谱联用检测海藻中砷形态%Determination of arsenic speciation in seaweeds using high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    高鹭; 董伟峰; 彭心婷; 史立娟; 李妍; 庞艳华; 徐静; 曹际娟

    2015-01-01

    目的:测定14种海藻样品中总砷和无机砷的含量,同时分析样品中6种砷形态。方法将海藻样品经过微波消解的前处理方法,通过电感耦合等离子体质谱(inductively coupled plasma mass spectrometry, ICP-MS)测定总砷含量;根据国标方法中无机砷检测的前处理方法,通过原子荧光光谱(atomic fluorescence spectrometry, AFS)测定无机砷含量;最后通过酸提的前处理方法,利用高效液相色谱-氢化物发生-原子荧光光谱法(high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry, HPLC-(UV)-HG-AFS)测定海藻样品中6种形态砷含量并与国标无机砷方法比较。结果14种海藻样品中总砷含量为0.038~46.2 mg/kg;无机砷含量为0.006~19.3 mg/kg;对HPLC-(UV)-HG-AFS仪器的优化和方法的摸索后,从海藻样品中主要测得的砷形态为As(III)、As(V)和DMA, MMA含量较少,没有测出AsB和 AsC。结论在砷形态较为复杂的海藻样品检测中,通过 HPLC-(UV)-HG-AFS 检测方法可以有效避免无机砷前处理中可能出现的有机砷向无机砷转变的现象,降低干扰,增加测试的准确性,更为具体地表现海藻样品中主要的砷形态含量。%Objective The content of total arsenic and inorganic arsenic were determined in 14 seaweeds and 6 kinds of arsenic species were determined at the same time. Methods The content of total arsenic was determined by inductively coupled plasma mass spectrometry (ICP-MS) after microwave digestion. According to the pretreatment method of national standard method, the content of inorganic arsenic was determined by atomic fluorescence spectrometry (AFS). The results of 6 arsenic species were studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry (HPLC-(UV)-HG-AFS) after acid extraction, which were compared with the national standard method. Results In 14

  12. Mercury speciation by high-performance liquid chromatography atomic fluorescence spectrometry using an integrated microwave/UV interface. Optimization of a single step procedure for the simultaneous photo-oxidation of mercury species and photo-generation of Hg{sup 0}

    Energy Technology Data Exchange (ETDEWEB)

    Quadros, Daiane P.C. de [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Campanella, Beatrice; Onor, Massimo; Bramanti, Emilia [National Research Council of Italy, C.N.R., Instituto di Chimica dei Composti Organo Metallici – ICCOM – UOS Pisa, Area della Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy); Borges, Daniel L.G. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); D' Ulivo, Alessandro, E-mail: dulivo@pi.iccom.cnr.it [National Research Council of Italy, C.N.R., Instituto di Chimica dei Composti Organo Metallici – ICCOM – UOS Pisa, Area della Ricerca, Via G. Moruzzi 1, 56124 Pisa (Italy)

    2014-11-01

    We described the hyphenation of photo-induced chemical vapor generation with high performance liquid chromatography–atomic fluorescence spectrometry (HPLC–AFS) for the quantification of inorganic mercury, methylmercury (MeHg) and ethylmercury (EtHg). In the developed procedure, formic acid in mobile phase was used for the photodecomposition of organomercury compounds and reduction of Hg{sup 2+} to mercury vapor under microwave/ultraviolet (MW/UV) irradiation. We optimized the proposed method studying the influence of several operating parameters, including the type of organic acid and its concentration, MW power, composition of HPLC mobile phase and catalytic action of TiO{sub 2} nanoparticles. Under the optimized conditions, the limits of detection were 0.15, 0.15 and 0.35 μg L{sup −1} for inorganic mercury, MeHg and EtHg, respectively. The developed method was validated by determination of the main analytical figures of merit and applied to the analysis of three certified reference materials. The online interfacing of liquid chromatography with photochemical-vapor generation–atomic fluorescence for mercury determination is simple, environmentally friendly, and represents an attractive alternative to the conventional tetrahydroborate (THB) system. - Highlights: • Inorganic and organic mercury were determined by photochemical vapor generation using a MW/UV photochemical reactor. • The optimized procedure has been applied to the speciation of Hg(II), MeHg and EtHg coupling HPLC with PVG–AFS. • The proposed method is simple, sensitive, and is established for mercury determination in biological materials.

  13. Determination of Trace Cadmium by Microwave Digestion-Hydride Generation Atomic Fluorescence Spectrometry%水及食品中微量镉的微波消解氢化物发生-原子荧光光谱测定法

    Institute of Scientific and Technical Information of China (English)

    张丽云; 张友谊; 刘淑晨

    2009-01-01

    Objective To develop a method for the determination of trace cadmium in drinking water or food using microwave digestion-hydride generation-atomic fluorescence spectrometry. Methods The microwave digestion method was used. Cobalt was added in the carrying liquid, the cadmium volatile matter was determined by atomic fluorescence spectrometry. Results The detection limit of this method was 0.1 ng/ml ,the liner range of cadmium was 0.1-100 ng/ml (r>0.999 3), the recovery rate was 96.9%-104.0%,RSD was 1.54%-2.03%. Conclusion The method is simple and rapid, with good sensitivity and selectivity, and it is applicable to the determination of trace cadmium in drinking water or food.%目的 探讨生活饮用水及食品中微量镉的微波消解氢化物发生原子荧光光谱测定法.方法 样品经微波消解后,以硼氢化钾为还原剂,稀盐酸为载流,加入钴离子,使镉与硼氢化钾反应生成镉的挥发性物质,以原子荧光光谱法进行测定.并探讨了实验条件.结果 方法的线性范围为0.1~100 ng/ml(r>0.999 3),检出限为0.1 ng/ml,回收率为96.9%~104.0%,RSD为1.54%~2.03%.结论 该方法灵敏度高、选择性好、操作方便、快速,适用于批量样品分析.

  14. 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.

  15. Atomic theories

    CERN Document Server

    Loring, FH

    2014-01-01

    Summarising the most novel facts and theories which were coming into prominence at the time, particularly those which had not yet been incorporated into standard textbooks, this important work was first published in 1921. The subjects treated cover a wide range of research that was being conducted into the atom, and include Quantum Theory, the Bohr Theory, the Sommerfield extension of Bohr's work, the Octet Theory and Isotopes, as well as Ionisation Potentials and Solar Phenomena. Because much of the material of Atomic Theories lies on the boundary between experimentally verified fact and spec

  16. Low-activity spectrometric gamma-ray logging technique for delineation of coal/rock interfaces in dry blast holes.

    Science.gov (United States)

    Asfahani, J; Borsaru, M

    2007-06-01

    A low-activity spectrometric gamma-ray logging technique is proposed in this paper as a sensitive tool for the delineation of coal/rock interfaces in dry blast holes. The advantages and superiority of this technique over traditional micro-density non-spectrometric gamma-ray tools are demonstrated.

  17. Advanced x-ray spectrometric techniques for characterization of nuclear materials: An overview of recent laboratory activities

    Science.gov (United States)

    Misra, N. L.

    2014-11-01

    Advancements in x-ray spectrometric techniques at different stages have made this technique suitable for characterization of nuclear materials with respect to trace/major element determinations and compositional uniformity studies. The two important features of total reflection x-ray fluorescence spectrometry: 1) requirement of very small amount of sample in ng level 2) multielement analytical capability, in addition to other features, make this technique very much suitable to nuclear materials characterization as most of the nuclear materials are radioactive and the radioactive waste generated and radiation hazards to the operator are minimum when such low amount of sample is used. Similarly advanced features of energy dispersive x-ray fluorescence e.g. better geometry for high flux, reduction in background due to application of radiation filters have made the measurements of samples sealed inside thin alkathene/PVC covers possible with good sensitivity. This approach avoids putting the instrument inside a glove box for measuring radioactive samples and makes the operation/maintenance of the instrument and analysis of the samples possible in easy and fast manner. This approach has been used for major element determinations in mixed uranium-plutonium samples. Similarly μ-XRF with brilliant and micro-focused excitation sources can be used for compositional uniformity study of reactor fuel pellets. A μ-XRF study using synchrotron light source has been made to assess the compositional uniformity of mixed uranium-thorium oxide pellets produced by different processes. This approach is simple as it does not involve any sample preparation and is non-destructive. A brief summary of such activities carried out in our laboratory in past as well as ongoing and planned for the future have been discussed in the present manuscript.

  18. High-Definition X-Ray Fluorescence: Applications

    OpenAIRE

    Gibson, Walter M.; Chen, Z W; Li, Danhong

    2008-01-01

    Energy dispersive X-ray fluorescence (EDXRF) is a well-established and powerful tool for nondestructive elemental analysis of virtually any material. It is widely used for environmental, industrial, pharmaceutical, forensic, and scientific research applications to measure the concentration of elemental constituents or contaminants. The fluorescing atoms can be excited by energetic electrons, ions, or photons. A particular EDXRF method, monochromatic microbeam X-ray fluorescence (MμEDXRF), has...

  19. High Definition X-Ray Fluorescence: Principles and Techniques

    OpenAIRE

    Chen, Z W; Gibson, Walter M.; Huang, Huapeng

    2008-01-01

    Energy dispersive X-ray fluorescence (EDXRF) is a well-established and powerful tool for nondestructive elemental analysis of virtually any material. It is widely used for environmental, industrial, pharmaceutical, forensic, and scientific research applications to measure the concentration of elemental constituents or contaminants. The fluorescing atoms can be excited by energetic electrons, ions, or photons. A particular EDXRF method, monochromatic microfocus X-ray fluorescence (MμEDXRF), ha...

  20. 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.

  1. Determination of cadmium and lead in human biological samples by spectrometric techniques: a review.

    Science.gov (United States)

    Lemos, Valfredo Azevedo; de Carvalho, Anaildes Lago

    2010-12-01

    The analysis of human biological samples, such as blood, urine, nails, and hair, is generally used for the verification of human exposure to toxic metals. In this review, various spectrometric methods for the determination of cadmium and lead in biological samples are discussed and compared. Several spectrometric techniques are presented and discussed with respect to various characteristics such as sensitivity, selectivity, and cost. Special attention is drawn to the procedures for digestion prior to the determination of cadmium and lead in hair, nails, blood, and urine.

  2. Fluorescence analysis of iodinated acetophenone derivatives.

    Science.gov (United States)

    Crivelaro, F; Oliveira, M R S; Lima, S M; Andrade, L H C; Casagrande, G A; Raminelli, C; Caires, A R L

    2015-03-15

    In the present paper the synthesis and optical characterization of iodinated acetophenone, 4-hydroxy-3-iodoacetophenone and 4-hydroxy-3,5-diiodoacetophenone obtained from 4-hydroxyacetophenone, were carried out. The optical features of iodinated molecules were determined by performing the UV-Vis absorption, fluorescence and thermal lens spectroscopies. The results showed that the optical properties of the 4-hydroxyacetophenone is altered when the iodine atom is inserted, as substituent, in the aromatic ring. Although it was determined that the optical feature was changed when one iodine atom was inserted in the aromatic ring (4-hydroxy-3-iodoacetophenone), the results revealed that emission behavior was strongly altered when two iodine atoms (4-hydroxy-3,5-diiodoacetophenone) were acting as substituents: the fluorescence quantum efficiency increases approximately 60%.

  3. Two-photon ionization of colliding atoms

    Energy Technology Data Exchange (ETDEWEB)

    Nayfeh, M.H.

    1977-09-01

    Semiclassical expressions of two-photon ionization of two colliding atoms are derived for a wide range of electromagnetic field intensity and detunings from the isolated atom line. The dependence of the ionization yield on the details of the interaction potential of the system is derived. This process promises an extremely sensitive method for studying line broadening on the far wing, especially when absorption or fluorescence becomes very weak.

  4. Studies concerning heavy metals bioaccumulation of wild edible mushrooms from industrial area by using spectrometric techniques.

    Science.gov (United States)

    Radulescu, Cristiana; Stihi, Claudia; Busuioc, Gabriela; Gheboianu, Anca Irina; Popescu, Ion V

    2010-05-01

    The aim of this work was to determine the heavy metal content of the fruiting bodies of four species of wild edible mushrooms and their respective substrates. The samples were collected from Dambovita County, Romania, at various distances from of a metal smelter, to asses the concentration of Cr, Mn, Fe, Ni, Cu, Zn, Se and Cd in the wild edible mushrooms and their substrate using Energy Dispersive X-ray Fluorescence (EDXRF) spectrometry together with Flame Atomic Absorption (FAAS) spectrometry. A quantitative evaluation of the relationship of element uptake by mushrooms from substrate was made by calculating the coefficient accumulation (K(a)). A high accumulation of Zn (K(a) range 1.01 to 2.01) was observed in mushrooms growing in the vicinity of the metal smelter.

  5. Atomic physics

    Energy Technology Data Exchange (ETDEWEB)

    Livingston, A.E.; Kukla, K.; Cheng, S. [Univ. of Toledo, OH (United States)] [and others

    1995-08-01

    In a collaboration with the Atomic Physics group at Argonne and the University of Toledo, the Atomic Physics group at the University of Notre Dame is measuring the fine structure transition energies in highly-charged lithium-like and helium-like ions using beam-foil spectroscopy. Precise measurements of 2s-2p transition energies in simple (few-electron) atomic systems provide stringent tests of several classes of current atomic- structure calculations. Analyses of measurements in helium-like Ar{sup 16+} have been completed, and the results submitted for publication. A current goal is to measure the 1s2s{sup 3}S{sub 1} - 1s2p{sup 3}P{sub 0} transition wavelength in helium-like Ni{sup 26+}. Measurements of the 1s2s{sup 2}S{sub 1/2} - 1s2p{sup 2}P{sub 1/2,3/2} transition wavelengths in lithium-like Kr{sup 33+} is planned. Wavelength and lifetime measurements in copper-like U{sup 63+} are also expected to be initiated. The group is also participating in measurements of forbidden transitions in helium-like ions. A measurement of the lifetime of the 1s2s{sup 3}S{sub 1} state in Kr{sup 34+} was published recently. In a collaboration including P. Mokler of GSI, Darmstadt, measurements have been made of the spectral distribution of the 2E1 decay continuum in helium-like Kr{sup 34+}. Initial results have been reported and further measurements are planned.

  6. Fundamentals of fluorescence and fluorescence microscopy.

    Science.gov (United States)

    Wolf, David E

    2013-01-01

    This chapter discusses the fundamental physics of fluorescence. The application of fluorescence to microscopy represents an important transition in the development of microscopy, particularly as it applies to biology. It enables quantitating the amounts of specific molecules within a cell, determining whether molecules are complexing on a molecular level, measuring changes in ionic concentrations within cells and organelles, and measuring molecular dynamics. This chapter also discusses the issues important to quantitative measurement of fluorescence and focuses on four of quantitative measurements of fluorescence--boxcar-gated detection, streak cameras, photon correlation, and phase modulation. Although quantitative measurement presents many pitfalls to the beginner, it also presents significant opportunities to one skilled in the art. This chapter also examines how fluorescence is measured in the steady state and time domain and how fluorescence is applied in the modern epifluorescence microscope.

  7. Quantitative MALDI tandem mass spectrometric imaging of cocaine from brain tissue with a deuterated internal standard.

    NARCIS (Netherlands)

    Pirman, D.A.; Reich, R.F.; Kiss, A.; Heeren, R.M.A.; Yost, R.A.

    2013-01-01

    Mass spectrometric imaging (MSI) is an analytical technique used to determine the distribution of individual analytes within a given sample. A wide array of analytes and samples can be investigated by MSI, including drug distribution in rats, lipid analysis from brain tissue, protein differentiation

  8. Terverticillate Penicillia studied by direct electrospray mass spectrometric profiling of crude extracts: I. Chemosystematics

    DEFF Research Database (Denmark)

    Smedsgaard, Jørn; Frisvad, Jens Christian

    1997-01-01

    A chemosystematic study of 339 isolates from all known terverticillate Penicillium taxa was performed using electrospray mass spectrometric analysis of extractable metabolites. The mass profiles were made by injecting crude plug extracts made from cultures grown on Czapek Yeast Autolysate agar (C...... to known secondary metabolites were, however, found in all mass profiles. (C) 1997 Elsevier Science Ltd....

  9. 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...

  10. Retrospective detection of exposure to organophosphorus anti-cholinesterases: Mass spectrometric analysis of phosphylated human butyrylcholinesterase

    NARCIS (Netherlands)

    Fidder, A.; Hulst, A.G.; Noort, D.; Ruiter, R. de; Schans, M.J. van der; Benschop, H.P.; Langenberg, J.P.

    2002-01-01

    In this paper a novel and general procedure is presented for detection of organophosphate-inhibited human butyrylcholinesterase (HuBuChE), which is based on electrospray tandem mass spectrometric analysis of phosphylated nonapeptides obtained after pepsin digestion of the enzyme. The utility of this

  11. 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

  12. The Atomic orbitals of the topological atom

    OpenAIRE

    Ramos-Cordoba, Eloy; Salvador Sedano, Pedro

    2013-01-01

    The effective atomic orbitals have been realized in the framework of Bader's atoms in molecules theory for a general wavefunction. This formalism can be used to retrieve from any type of calculation a proper set of orthonormalized numerical atomic orbitals, with occupation numbers that sum up to the respective Quantum Theory of Atoms in Molecules (QTAIM) atomic populations. Experience shows that only a limited number of effective atomic orbitals exhibit significant occupation numbers. These c...

  13. Principles of fluorescence techniques

    CERN Document Server

    2016-01-01

    Fluorescence techniques are being used and applied increasingly in academics and industry. The Principles of Fluorescence Techniques course will outline the basic concepts of fluorescence techniques and the successful utilization of the currently available commercial instrumentation. The course is designed for students who utilize fluorescence techniques and instrumentation and for researchers and industrial scientists who wish to deepen their knowledge of fluorescence applications. Key scientists in the field will deliver theoretical lectures. The lectures will be complemented by the direct utilization of steady-state and lifetime fluorescence instrumentation and confocal microscopy for FLIM and FRET applications provided by leading companies.

  14. Reviews in fluorescence 2010

    CERN Document Server

    Geddes, Chris D

    2011-01-01

    ""Reviews in Fluorescence 2010"", the seventh volume of the book serial from Springer, serves as a comprehensive collection of current trends and emerging hot topics in the field of fluorescence and closely related disciplines. It summarizes the year's progress in fluorescence and its applications, with authoritative analytical reviews specialized enough to be attractive to professional researchers, yet also appealing to the wider audience of scientists in related disciplines of fluorescence. ""Reviews in Fluorescence"" offers an essential reference material for any lab working in the fluoresc

  15. 氢化物原子荧光光谱法同时测定血液透析用水中的砷和锑%Simultaneous determination of arsenic and antimony in blood dialysis water by hydride atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    汪洋; 邵丽华; 魏滨; 何漪

    2011-01-01

    Objective:To establish a method for the simultaneous determination of arsenic and antimony in blood dialysis water by hydride atomic fluorescence spectrometry. Methods: The working condition of the determination were studied and optimized for the simultaneous determination of arsenic and antimony in blood dialysis water by hydride atomic fluorescence spectrometry.Results: The detection limits of this method were found to be 0.40 μg/L for arsenic and 0.50 μg/L for antimony, and the RSD were in the range of 2.2% ~ 4.2% for arsenic and 3.2% ~ 5.3% for antimony. The recovery tates of standard spiking for arsenic and antimony were in the range of 94.0% ~ 101.2% and 98.9% ~ 103.6%, respectively. Conclusion: The method is sensitive, accurate and rapid. It can be adopted for simultaneous determination of arsenic and antimony in blood dialysis water.%目的:建立一种氢化物原子荧光光谱法同时测定血液透析用水中的砷和锑的方法.方法:优化测定条件,采用氢化物原子荧光光谱法同时测定血液透析用水中的砷和锑.结果:砷和锑的检出限、相对标准偏差、回收率分别为:0.40μg/L和0.50 μg/L;2.2%~4.2%和3.2%~5.3%;94.0%~101.2%和98.9%~103.6%.结论:本方法灵敏度高,准确、快捷,能同时测定血液透析用水中的砷和锑,省时、省力.

  16. 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.

  17. Atom Skimmers and Atom Lasers Utilizing Them

    Science.gov (United States)

    Hulet, Randall; Tollett, Jeff; Franke, Kurt; Moss, Steve; Sackett, Charles; Gerton, Jordan; Ghaffari, Bita; McAlexander, W.; Strecker, K.; Homan, D.

    2005-01-01

    Atom skimmers are devices that act as low-pass velocity filters for atoms in thermal atomic beams. An atom skimmer operating in conjunction with a suitable thermal atomic-beam source (e.g., an oven in which cesium is heated) can serve as a source of slow atoms for a magneto-optical trap or other apparatus in an atomic-physics experiment. Phenomena that are studied in such apparatuses include Bose-Einstein condensation of atomic gases, spectra of trapped atoms, and collisions of slowly moving atoms. An atom skimmer includes a curved, low-thermal-conduction tube that leads from the outlet of a thermal atomic-beam source to the inlet of a magneto-optical trap or other device in which the selected low-velocity atoms are to be used. Permanent rare-earth magnets are placed around the tube in a yoke of high-magnetic-permeability material to establish a quadrupole or octupole magnetic field leading from the source to the trap. The atoms are attracted to the locus of minimum magnetic-field intensity in the middle of the tube, and the gradient of the magnetic field provides centripetal force that guides the atoms around the curve along the axis of the tube. The threshold velocity for guiding is dictated by the gradient of the magnetic field and the radius of curvature of the tube. Atoms moving at lesser velocities are successfully guided; faster atoms strike the tube wall and are lost from the beam.

  18. Fluorescence correlation spectroscopy

    NARCIS (Netherlands)

    Hink, M.A.; Verveer, P.J.

    2015-01-01

    Fluorescence fluctuation spectroscopy techniques allow the quantification of fluorescent molecules present at the nanomolar concentration level. After a brief introduction to the technique, this chapter presents a protocol including background information in order to measure and quantify the molecul

  19. Experimental Investigation of Excited-State Lifetimes in Atomic Ytterbium

    Energy Technology Data Exchange (ETDEWEB)

    Bowers, C.J.; Budker, D.; Commins, E.D.; DeMille, D.; Freedman, S.J.; Nguyen, A.-T.; Shang, S.-Q.; /UC, Berkeley; Zolotorev, M.; /SLAC

    2011-11-15

    Lifetimes of 21 excited states in atomic Yb were measured using time-resolved fluorescence detection following pulsed laser excitation. The lifetime of the 4f{sup 14}5d6s {sup 3}D{sub 1} state, which is of particular importance for a proposed study of parity nonconservation in atoms, was measured to be 380(30) ns.

  20. Electrochemical hydride generation atomic fluorescence spectrometry with a polyanline modified electrode for detection of tin%聚苯胺修饰电极-电化学氢化物发生原子荧光光谱法测定食品中锡含量

    Institute of Scientific and Technical Information of China (English)

    姜宪娟; 淦五二

    2012-01-01

    An electrochemical hydride generation (EC-HG) system with a polyaniline modified electrode (Pan-ME) as cathode material was developed for Sn ( Ⅳ) determination by couped with atomic fluorescence spectrometry. The electrochemical hydride generation efficiency for Sn (Ⅳ) was improved evidently as the Pan membrane could obstruct the aggradation of Sn atom on cathode surface and facilitate the hydride generation. The effects of experimental parameters and interferences have been studied. The limit of detection ( LOD) was 1. 2 ng/mL (3σ) and the relative standard deviation (RSD) was 2. 3% for eleven consecutive measurements of 50 ng/mL Sn(IV) standard solution.%运用以聚苯胺修饰的石墨电极为阴极的电化学氢化物发生装置实现了锡元素的电化学氢化物发生.在电极表面聚合一层聚苯胺,能够有效地提高锡元素的电化学氢化物发生效率,通过与原子荧光光谱仪联用,成功地测定了食品中的锡含量.本工作对各种实验参数和干扰情况进行了详细研究.方法对锡的检出限为1.2 ng/mL(3σ);样品分析精密度(RSD)为2.3% (50 ng/mL,n=11).

  1. Safe biodegradable fluorescent particles

    Science.gov (United States)

    Martin, Sue I.; Fergenson, David P.; Srivastava, Abneesh; Bogan, Michael J.; Riot, Vincent J.; Frank, Matthias

    2010-08-24

    A human-safe fluorescence particle that can be used for fluorescence detection instruments or act as a safe simulant for mimicking the fluorescence properties of microorganisms. The particle comprises a non-biological carrier and natural fluorophores encapsulated in the non-biological carrier. By doping biodegradable-polymer drug delivery microspheres with natural or synthetic fluorophores, the desired fluorescence can be attained or biological organisms can be simulated without the associated risks and logistical difficulties of live microorganisms.

  2. 工作场所空气中汞及其化合物的原子荧光光谱测定法%Atomic fluorescence spectrometry determination of mercury and its compounds in workplace air

    Institute of Scientific and Technical Information of China (English)

    刘小娟; 张彩霞; 王晓红

    2012-01-01

    The standard curve, sample processing of GBZ / T 160. 14 - 2004 "toxic substances in workplace air-determination of mercury and its compounds" were improved for the accuracy of measurement. The method standard curve range was 0. 002 - 0. 014μg /mL, the correlation coefficient r = 0. 9994, regression equation If=71424C+5. 7623. High medium and low concentration of the standard precision of 1. 9%, 4. 1% , 4. 9%. The detection limit was 0. 001 spiked recoveries in the range 92% to 98%. The results showed that the processing of samples and standard curve preparation should note that glass pickling and to avoid contamination after acid with potassium borohydride solution soak, and eliminate pollution. Reducing agent is currently using the existing service. The detector can choose to replace contaminated piping and quartz furnace soak with aqua regia (atomizer).%本文在标准曲线、样品处理方面对GBZ/T 160.14-2004《工作场所空气中有毒物质测定 汞及其化合物》进行改进,提高了测量的准确性.标准曲线范围0.002~0.014 μg/mL,相关系数r=0.9994,回归方程If=71424C+5.7623.高、中、低浓度标准的精密度分别为1.9%、4.1%、4.9%.检出限为0.001 μg/mL,加标回收率范围92%~98%.样品的处理及标准益线的配制应注意玻璃器皿的酸洗和避免污染,酸洗后用硼氢化钾溶液浸泡一下,消除污染.还原剂现用现配.检测器被污染可更换管路或用王水浸泡清洗石英炉(原子化器).

  3. Interaction of norfloxacin with bovine serum albumin studied by different spectrometric methods; displacement studies, molecular modeling and chemometrics approaches

    Energy Technology Data Exchange (ETDEWEB)

    Naseri, Abdolhossein, E-mail: a_naseri@tabrizu.ac.ir [Departments of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51666-16471 (Iran, Islamic Republic of); Hosseini, Soheila [Departments of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz 51666-16471 (Iran, Islamic Republic of); Rasoulzadeh, Farzaneh [Drug Applied Research Center, Tabriz University of Medical Sciences, Tabriz 51644-14766 (Iran, Islamic Republic of); Rashidi, Mohammad-Reza [Research Center for Pharmaceutical Nanotechnology, Tabriz University of Medical Sciences, Tabriz 51644-14766 (Iran, Islamic Republic of); Zakery, Maryam; Khayamian, Taghi [Department of Chemistry, College of Chemistry, Isfahan University of Technology, Isfahan 84154 (Iran, Islamic Republic of)

    2015-01-15

    Serum albumins as major target proteins can bind to other ligands leading to alteration of their pharmacological properties. The mechanism of interaction between norfloxacin (NFLX) with bovine serum albumin (BSA) was investigated. Fuorescence quenching of serum albumin by this drug was found to be a static quenching process. The binding sites number, n, apparent binding constant, K, and thermodynamic parameters were calculated at different temperatures. The distance, r, between donor, BSA, and acceptor, NFLX, was calculated according to the Forster theory of non-radiation energy transfer. Also binding characteristics of NFLX with BSA together with its displacement from its binding site by kanamycin and effect of common metal ions on binding constant were investigated by the spectroscopic methods. The conformational change in the secondary structure of BSA upon interaction with NFLX was investigated qualitatively from synchronous fluorescence spectra, Fourier Transform Infrared (FTIR) and circular dichroism (CD) spectrometric methods. Molecular docking studies were performed to obtain information on the possible residues involved in the interaction process and changes in accessible surface area of the interacting residues. The results showed that the conformation of BSA changed in the presence of NFLX. For the first time, displacement studies were used for this interaction; displacement studies showed that NFLX was displaced by phenylbutazon and ketoprofen but was not displaced by ibuprofen indicating that the binding site of NFLX on albumin was site I. In addition a powerful chemometrics method, multivariate curve resolution-alternating least square, was used for resolution of spectroscopic augmented data obtained in two different titration modes in order to extract spectral information regardless of spectral overlapping of components. - Highlights: • Interaction between norfloxacin and BSA is studied by spectral methods. • Chemometrics methods are used to

  4. Atomic magnetometer

    Science.gov (United States)

    Schwindt, Peter [Albuquerque, NM; Johnson, Cort N [Albuquerque, NM

    2012-07-03

    An atomic magnetometer is disclosed which uses a pump light beam at a D1 or D2 transition of an alkali metal vapor to magnetically polarize the vapor in a heated cell, and a probe light beam at a different D2 or D1 transition to sense the magnetic field via a polarization rotation of the probe light beam. The pump and probe light beams are both directed along substantially the same optical path through an optical waveplate and through the heated cell to an optical filter which blocks the pump light beam while transmitting the probe light beam to one or more photodetectors which generate electrical signals to sense the magnetic field. The optical waveplate functions as a quarter waveplate to circularly polarize the pump light beam, and as a half waveplate to maintain the probe light beam linearly polarized.

  5. 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.

  6. CANAS '01 - Colloquium analytical atomic spectroscopy; CANAS '01 - Colloquium Analytische Atomspektroskopie. Programm. Kurzfassungen der Vortraege und Poster

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2001-07-01

    The main topics of the meeting on analytical atom spectroscopy were: optical atom spectrometry, x-ray fluorescence analysis, absorption spectroscopy, icp mass spectroscopy, trace analysis, sampling, sample preparation and quality assurance.

  7. Total reflection X-ray fluorescence spectrometric determination of elements in water hyacinth from the Lerma River

    Energy Technology Data Exchange (ETDEWEB)

    Tejeda, S. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Instituto Tecnologico de Toluca, Division de Estudios de Posgrado e Investigacion, Apartado Postal 890, Metepec, C.P. 52149 (Mexico); Zarazua, G., E-mail: graciela.zarazua@inin.gob.m [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Avila-Perez, P. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Instituto Tecnologico de Toluca, Division de Estudios de Posgrado e Investigacion, Apartado Postal 890, Metepec, C.P. 52149 (Mexico); Carapia-Morales, L. [Instituto Nacional de Investigaciones Nucleares, Gerencia de Ciencias Ambientales, Apartado Postal 18-1027, Mexico D.F., C.P. 11801 (Mexico); Martinez, T. [Universidad Nacional Autonoma de Mexico, Facultad de Quimica, Mexico D.F. (Mexico)

    2010-06-15

    The Lerma River is one of the most polluted body water in Mexico. For this reason, only the highly resistant organisms such as water hyacinth are able to reproduce in this river. The aim of this work was to evaluate the concentration of K, S, Fe, Ca, Mn, Ti, Zn, Sr, Rb, Cu, Cr, Ni, Pb and Br in roots of water hyacinth (Eichhornia crassipes) from the Lerma River. The samples were collected from five sites in the river and analyzed in triplicate using a TXRF Spectrometer 'TX-2000 Ital Structures' with a Si(Li) detector and a resolution of 140 eV (FWHM) at Mn K{alpha}. A Mo tube (40 kV, 30 mA) with 17.4 KeV excitation energy was used for a counting time of 500 s. Results show that the average metal concentration in the water hyacinth roots decrease in the following order: K (9698.2 {mu}g/g) > S (7593.3 {mu}g/g) > Fe (4406.6 {mu}g/g) > Ca (2601.8 {mu}g/g) > Mn (604.2 {mu}g/g) > Ti (230.7 {mu}g/g) > Zn (51.65 {mu}g/g) > Sr (43.55 {mu}g/g) > Rb (18.61 {mu}g/g) > Cu (12.78 {mu}g/g) > Cr (6.45 {mu}g/g) > Ni (4.68 {mu}g/g) > Pb (4.32 {mu}g/g) > Br (4.31 {mu}g/g) and the bioconcentration factors in the water hyacinth decrease in the sequence: Ti > Fe > Mn > Cu > Ni > Zn > S > Pb > Rb > K > Cr > Sr > Br > Ca. The concentrations in roots of water hyacinth reflect the high pollution level of the river.

  8. Total reflection X-ray fluorescence spectrometric determination of elements in water hyacinth from the Lerma River

    Science.gov (United States)

    Tejeda, S.; Zarazúa, G.; Ávila-Pérez, P.; Carapia-Morales, L.; Martínez, T.

    2010-06-01

    The Lerma River is one of the most polluted body water in Mexico. For this reason, only the highly resistant organisms such as water hyacinth are able to reproduce in this river. The aim of this work was to evaluate the concentration of K, S, Fe, Ca, Mn, Ti, Zn, Sr, Rb, Cu, Cr, Ni, Pb and Br in roots of water hyacinth ( Eichhornia crassipes) from the Lerma River. The samples were collected from five sites in the river and analyzed in triplicate using a TXRF Spectrometer 'TX-2000 Ital Structures' with a Si(Li) detector and a resolution of 140 eV (FWHM) at Mn Kα. A Mo tube (40 kV, 30 mA) with 17.4 KeV excitation energy was used for a counting time of 500 s. Results show that the average metal concentration in the water hyacinth roots decrease in the following order: K (9698.2 µg/g) > S (7593.3 µg/g) > Fe (4406.6 µg/g) > Ca (2601.8 µg/g) > Mn (604.2 µg/g) > Ti (230.7 µg/g) > Zn (51.65 µg/g) > Sr (43.55 µg/g) > Rb (18.61 µg/g) > Cu (12.78 µg/g) > Cr (6.45 µg/g) > Ni (4.68 µg/g) > Pb (4.32 µg/g) > Br (4.31 µg/g) and the bioconcentration factors in the water hyacinth decrease in the sequence: Ti > Fe > Mn > Cu > Ni > Zn > S > Pb > Rb > K > Cr > Sr > Br > Ca. The concentrations in roots of water hyacinth reflect the high pollution level of the river.

  9. High Atom Number in Microsized Atom Traps

    Science.gov (United States)

    2015-12-14

    Final Performance Report on ONR Grant N00014-12-1-0608 High atom number in microsized atom traps for the period 15 May 2012 through 14 September...TYPE Final Technical Report 3. DATES COVERED (From - To) 05/15/2012-09/14/2012 4. TITLE AND SUBTITLE High atom number in microsized atom traps...forces for implementing a small-footprint, large-number atom -chip instrument. Bichromatic forces rely on absorption and stimulated emission to produce

  10. 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.

  11. 氢化物发生-非色散原子荧光光谱法同时测定金精矿中痕量铋和汞%Simultaneous determination of trace bismuth and mercury in gold concentrates by hydride generation-nondispersive atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    马熠罡

    2012-01-01

    The method of simultaneous determination of trace bismuth and mercury in gold concentrates by hydride generation-nondispersive atomic fluorescence spectrometry was proposed. The samples were digested by HNO3/HCI and then some references were marked by potassium thiocyanate and thiourea. Calculated the detection limits are 5.6 mg/L and 0. 7 mg/L. The method detection limits are 0. 13 μg/g and 0.012 μg/g,and the precision were 1.2% and 0.6% ,respectively.%采用HNO3/HCl消解,以硫氰化钾掩蔽金,硫脲掩蔽杂质等手段,建立王水消解-双道氢化物发生原子荧光光谱同时测定金精矿中铋和汞含量的新方法.计算出Bi和Hg的检出限分别为5.6,0.7 mg/L,方法的检出限分别为0.13μg/g和0.012 μg/g,精密度分别为1.2%和0.6%.

  12. 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

  13. 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.

  14. The prediction of paper properties from spectrometric data with machine learning

    OpenAIRE

    Jakovac, Alen

    2011-01-01

    In this thesis we present a solution for the problem of predicting the chemical and physical properties of paper from spectrometric data. We used a data set that consists of over 1000 samples of paper. For each sample 15 chemical and physical properties and its near-infrared spectra were measured. We used the following machine learning methods to predict the properties of paper: linear regression, pace regression, a nearest neighbor-based model, regression trees, a support vector machine, ...

  15. Remote mass spectrometric sampling of electrospray- and desorption electrospray-generated ions using an air ejector.

    Science.gov (United States)

    Dixon, R Brent; Bereman, Michael S; Muddiman, David C; Hawkridge, Adam M

    2007-10-01

    A commercial air ejector was coupled to an electrospray ionization linear ion trap mass spectrometer (LTQ) to transport remotely generated ions from both electrospray (ESI) and desorption electrospray ionization (DESI) sources. We demonstrate the remote analysis of a series of analyte ions that range from small molecules and polymers to polypeptides using the AE-LTQ interface. The details of the ESI-AE-LTQ and DESI-AE-LTQ experimental configurations are described and preliminary mass spectrometric data are presented.

  16. Spectrometric and Voltammetric Analysis of Urease – Nickel Nanoelectrode as an Electrochemical Sensor

    OpenAIRE

    Rene Kizek; Josef Zehnalek; Martin Adamek; Katerina Klosova; Ales Horna; Libuse Trnkova*; Michal Masarik; Dalibor Huska; Olga Krystofova; Vojtech Adam; Jan Hradecky; Jaromir Hubalek

    2007-01-01

    Urease is the enzyme catalyzing the hydrolysis of urea into carbon dioxide and ammonia. This enzyme is substrate- specific, which means that the enzyme catalyzes the hydrolysis of urea only. This feature is a basic diagnostic criterion used in the determination of many bacteria species. Most of the methods utilized for detection of urease are based on analysis of its enzyme activity - the hydrolysis of urea. The aim of this work was to detect urease indirectly by spectrometric method and dire...

  17. Mass spectrometric identification of proteins and characterization of their post-translational modifications in proteome analysis

    DEFF Research Database (Denmark)

    Roepstorff, P; Larsen, Martin Røssel

    2001-01-01

    dominant strategies for identification of proteins from gels based on peptide mass spectrometric fingerprinting and partial sequencing by mass spectrometry are described. After identification of the proteins the next challenge in proteome analysis is characterization of their post-translational...... modifications. The general problems associated with characterization of these directly from gel separated proteins are described and the current state of art for the determination of phosphorylation, glycosylation and proteolytic processing is illustrated....

  18. Heterogeneous nuclear ribonucleoproteins C1/C2 identified as autoantigens by biochemical and mass spectrometric methods

    DEFF Research Database (Denmark)

    Heegaard, N H; Larsen, Martin Røssel; Muncrief, T

    2000-01-01

    The antigenic specificity of an unusual antinuclear antibody pattern in three patient sera was identified after separating HeLa-cell nuclear extracts by two-dimensional (2D) gel electrophoresis and localizing the antigens by immunoblotting with patient serum. Protein spots were excised from the 2......-separation methods and mass-spectrometric peptide mapping in combination with database searches are powerful tools in the identification of novel autoantigen specificities....

  19. 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.

  20. Spectrometric methods used in the calibration of radiodiagnostic measuring instruments

    Energy Technology Data Exchange (ETDEWEB)

    De Vries, W. [Rijksuniversiteit Utrecht (Netherlands)

    1995-12-01

    Recently a set of parameters for checking the quality of radiation for use in diagnostic radiology was established at the calibration facility of Nederlands Meetinstituut (NMI). The establishment of the radiation quality required re-evaluation of the correction factors for the primary air-kerma standards. Free-air ionisation chambers require several correction factors to measure air-kerma according to its definition. These correction factors were calculated for the NMi free-air chamber by Monte Carlo simulations for monoenergetic photons in the energy range from 10 keV to 320 keV. The actual correction factors follow from weighting these mono-energetic correction factors with the air-kerma spectrum of the photon beam. This paper describes the determination of the photon spectra of the X-ray qualities used for the calibration of dosimetric instruments used in radiodiagnostics. The detector used for these measurements is a planar HPGe-detector, placed in the direct beam of the X-ray machine. To convert the measured pulse height spectrum to the actual photon spectrum corrections must be made for fluorescent photon escape, single and multiple compton scattering inside the detector, and detector efficiency. From the calculated photon spectra a number of parameters of the X-ray beam can be calculated. The calculated first and second half value layer in aluminum and copper are compared with the measured values of these parameters to validate the method of spectrum reconstruction. Moreover the spectrum measurements offer the possibility to calibrate the X-ray generator in terms of maximum high voltage. The maximum photon energy in the spectrum is used as a standard for calibration of kVp-meters.

  1. The atomic orbitals of the topological atom.

    Science.gov (United States)

    Ramos-Cordoba, Eloy; Salvador, Pedro; Mayer, István

    2013-06-07

    The effective atomic orbitals have been realized in the framework of Bader's atoms in molecules theory for a general wavefunction. This formalism can be used to retrieve from any type of calculation a proper set of orthonormalized numerical atomic orbitals, with occupation numbers that sum up to the respective Quantum Theory of Atoms in Molecules (QTAIM) atomic populations. Experience shows that only a limited number of effective atomic orbitals exhibit significant occupation numbers. These correspond to atomic hybrids that closely resemble the core and valence shells of the atom. The occupation numbers of the remaining effective orbitals are almost negligible, except for atoms with hypervalent character. In addition, the molecular orbitals of a calculation can be exactly expressed as a linear combination of this orthonormalized set of numerical atomic orbitals, and the Mulliken population analysis carried out on this basis set exactly reproduces the original QTAIM atomic populations of the atoms. Approximate expansion of the molecular orbitals over a much reduced set of orthogonal atomic basis functions can also be accomplished to a very good accuracy with a singular value decomposition procedure.

  2. "Bohr's Atomic Model."

    Science.gov (United States)

    Willden, Jeff

    2001-01-01

    "Bohr's Atomic Model" is a small interactive multimedia program that introduces the viewer to a simplified model of the atom. This interactive simulation lets students build an atom using an atomic construction set. The underlying design methodology for "Bohr's Atomic Model" is model-centered instruction, which means the central model of the…

  3. Biosorption of platinum and palladium for their separation/preconcentration prior to graphite furnace atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Godlewska-Zylkiewicz, Beata E-mail: bgodlew@uwb.edu.pl

    2003-08-15

    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 (<2%), improved efficiency of platinum retention on the column (93.3{+-}1.6%), is less laborious and less time consuming. The best recovery of biosorbed metals from column (87.7{+-}3.3% for platinum and 96.8{+-}1.1 for palladium) was obtained with solution of 0.3 mol l{sup -1} thiourea in 1 mol l{sup -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.

  4. 40 CFR Appendix C to Part 136 - Inductively Coupled Plasma-Atomic Emission Spectrometric Method for Trace Element Analysis of...

    Science.gov (United States)

    2010-07-01

    ... 2 are intended for use only as a rudimentary guide for the indication of potential spectral... and repeat the calibration. 13.Precision and Accuracy 13.1An interlaboratory study of metal analyses... in Academic Chemistry Laboratories, American Chemical Society Publication, Committee on...

  5. Development of a fast atom bombardment tandem mass spectrometric screening method for alkyl-ended oligomeric biguanides

    Science.gov (United States)

    Monaghan, J. J.; Morden, W. E.

    1992-12-01

    The FAB-MS and FAB-MS---MS behaviour of a series of "alkyl-ended" oligomeric biguanides has been studied. MS---MS product ion scans showed that fragmentation of these species occurred by predictable cleavages of the biguanide chains. Results are presented from a number of MS---MS precursor ion and neutral loss scans studied in an attempt to develop a screening method for biguanides in complex mixtures. The most effective of these scans is shown to be the neutral loss of the N-alkylguanidine molecule. Use of this scan is demonstrated for a mixture of oligomeric biguanides.

  6. An atomic absorption spectrometric method for the determination of phosphorus in foodstuffs using the bismuth phosphomolybdate complex

    Directory of Open Access Journals (Sweden)

    LJILJANA V. MIHAJLOVIC

    2000-06-01

    Full Text Available A new indirect AAS method using the bismuth phosphomolybdate complex for the determination of phosphorus in foodstuffs is suggested. The bismuth phosphomolybdate complex in acid medium was extacted with isobutyl methylketone and the phosphorus was determined through bismuth in an air/acetylene flame by utilising the 223.06 nm resonance line of bismuth. The interference caused by antimony and titanium can be neglected in the presence of excess of bismuth. The detection limit of the method is 0.008 mg/mL of phosphorus.

  7. Metastable states' population of uranium atoms produced by electron-beam heating

    Energy Technology Data Exchange (ETDEWEB)

    Ohba, Hironori; Shibata, Takemasa [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment; Nishimura, Akihiko; Ogura, Koichi [Japan Atomic Energy Research Inst., Kansai Research Establishment, Advanced Photon Research Center, Kyoto (Japan)

    2000-08-01

    The metastable states' population densities of uranium atoms produced by electron-beam heating were measured by the laser induced fluorescence method. The atomic excitation temperature derived from the metastable state distribution was lower than the evaporation surface temperature. With increasing deposition rate, the atomic excitation temperature decreased to about 2000 K. (author)

  8. Defect-free atom arrays on demand

    Science.gov (United States)

    Levine, Harry; Bernien, Hannes; Keesling, Alex; Anschuetz, Eric; Senko, Crystal; Vuletic, Vladan; Greiner, Markus; Endres, Manuel; Lukin, Mikhail

    2016-05-01

    Arrays of neutral, trapped atoms have proven to be an extraordinary platform for studying quantum many-body physics and implementing quantum information protocols. Conventional approaches to generate such arrays rely on loading atoms into optical lattices and require elaborate experimental control. An alternative, simpler approach is to load atoms into individual optical tweezers. However, the probabilistic nature of the loading process limits the size of the arrays to small numbers of atoms. Here we present a new method for assembling defect-free arrays of large numbers of atoms. Our technique makes use of an array of tightly focused optical tweezers generated by an acousto-optic deflector. The positions of the traps can be dynamically reconfigured on a sub-millisecond timescale. With single-site resolved fluorescence imaging, we can identify defects in the atom array caused by the probabilistic loading process and rearrange the trap positions in response. This will enable us to generate defect-free atom arrays on demand. We discuss our latest results towards reaching this goal along with schemes to implement long-range interactions between atoms in the array. Now at Caltech.

  9. 氢化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)%Direct Determination of Water-Soluble Antimony(Ⅲ) and Antimony(Ⅴ) in Soil by Hydride Generation Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    于兆水; 张勤

    2009-01-01

    在HCl介质中,Sb(Ⅲ)和Sb(Ⅴ)在氢化物发生过程中的化学反应效率不同,通过测定经还原剂还原后和还原前Sb的荧光强度,求解联立方程计算出Sb(Ⅲ)和Sb(Ⅴ)的含量,据此建立了氧化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)方法,操作简便,实用性强.考察了 HCl浓度和KBH_4浓度对Sb(Ⅲ)和Sb(Ⅴ)测定灵敏度的影响以及共存元素的干扰情况,并比较了丽种还原剂对Sb(Ⅴ)的还原效果.方法检出限为Sb(Ⅲ)1.11 ng·g~(-1),Sb(Ⅴ)1.57 ng·g~(-1).加标回收试验表明方法准确、可靠.%A simple, rapid and useful method for the determination of water-soluble antimony( Ⅲ ) and antimony(Ⅴ) in soil was established using hydride generation atomic fluorescence spectrometry. The method was based on the different chemical reaction efficiency between Sb( Ⅲ ) and Sb( Ⅴ ) with KBH_4 in the media of HCL The amounts of Sb( Ⅲ) and Sb( Ⅴ ) can be obtained through measuring antimony fluorescence intensities before and after reduction with reductant. The effects of HCI and KBH_4 on the sensitivities of Sb(Ⅲ) and Sb(Ⅴ) were investigated, and the interferences from coexistent elements were studied. The re-duction efficiencies of both reductants were compared. The detection limits of the method were 1.11 ng·g~(-1) for Sb( Ⅲ ) and 1.57 ng·g~(-1) for Sb( Ⅴ ). The accuracy of the method was verified by recovery experiments on spiked real soil samples.

  10. Determination of inorganic arsenic in coal by hydride generation atomic fluorescence spectrometry combined with ultrasonic extraction%超声提取-顺序注射氢化物发生-原子荧光光谱法测定煤中无机砷

    Institute of Scientific and Technical Information of China (English)

    王长芹; 刘贵勤

    2011-01-01

    A determination method of inorganic arsemc in coal was established by sequence injection hydride generation-atomic fluorescence spectrometry ( HG-AFS) , after the ultrasonic extraction with 6 mol/L HCl as extraction reagent. The ultrasonic extraction conditions were optimized, including extraction reagent, time and temperature. Under the optimized experimental condition, arsemc in concentration range of 0. 20-100 μg/L showed linearity to the fluorescence intensity with correlation coefficient of 0. 999 7. The detection limit of arsenic was 0. 025 μg/L. The relative standard deviation (RSD) for 10 μg/L As was 0. 9 % (n=11). The proposed method has been applied to the analysis of coal fly ash component analysis certified reference material (GBW08401) and coal samples with recoveries of 95%-102 %, and the result of GBW08401 was consist with the certified value.%利用6 mol/L盐酸作为提取试剂,样品经超声提取后,用顺序注射氢化物发生-原子荧光光谱法测定煤中无机砷的含量.对超声提取条件(提取试剂浓度、时间、温度)进行了优化.在优化的实验条件下,砷的浓度在0.20~100μg/L范围内与荧光强度呈线性关系,相关系数为0.999 7,砷的检出限为0.025μg/L,对10 μg/L砷标准溶液进行重复11次测量,得出相对标准偏差(RSD)为0.9%.用该法对煤飞灰成分分析标准物质GBW08401和煤样进行分析,测得回收率在95%~102%之间,标准样品的测定值和认定值相符.

  11. 甲基异丁基甲酮萃取—氢化物发生原子荧光光谱法测定锑锭和氧化锑中汞%Determination of mercury in antimony ingot and antimony oxide by methyl isobutyl ketone extraction-hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    陆建平; 谭芳维; 石建荣

    2012-01-01

    After the samples were dissolved in aqua regia/HBr and tartaric acid was added to mask antimony, then mercury in antimony ingot and antimony oxide was extracted into the organic phase with methyl isobutyl ketone (MIBK) and determined by organic phase injection-intermittent flow injection atomic fluorescence spectrometry. Sample dissolution methods and interferences caused by coexisting ions were investigated, and instrument working conditions, extraction conditions, acidity and other factors were optimized. The results showed that under optimal conditions, the mercury content within the range of 0. 02 to 50 μg/L was in good linear relationship, and the detection limit was 0. 013 jxg/L. This method was applied to the actual antimony ingot and antimony oxide sample analysis. It was found that the results were consistent with those obtained by inductive coupled plasma atomic emission spectrometry with relative standard deviations (RSDs, n = 6) of 0. 65%-2. 4% and recoveries of 94 %-99%.%采用王水/HBr溶解样品,酒石酸掩蔽锑,用甲基异丁基甲酮(MIBK)将汞萃取到有机相中,建立了有机相进样—断续流动注射原子荧光光谱法测定锑锭和氧化锑中汞含量的方法.研究了溶样方法和共存离子可能引起的干扰,优化了仪器工作条件、萃取条件、酸度及其他影响因素.结果表明,在最佳条件下,汞含量在0.02~50 μg/L范围内线性关系良好,方法检出限为0.013 μg/L.将方法应用于锑锭和氧化锑实际样品分析,测得结果与电感耦合等离子体原子发射光谱法一致,相对标准偏差(RSD,n=6)在0.65%~2.4%之间,加标回收率为94%~99%.

  12. Strong Correlation of Fluorescence Photons without Quantum Interference

    Institute of Scientific and Technical Information of China (English)

    HU Xiang-Ming; WANG Fei

    2007-01-01

    It has been predicted that a driven three-level V atom can emit strongly correlated fluorescence photons in the presence of quantum interference. Here we examine the effects of quantum interference on the intensity correlation of fluorescence photons emitted from a driven three-level A atom. Unexpectedly, strong correlation occurs without quantum interference. The quantum interference tends to reduce the correlation function to a normal level. The essential difference between these two cases is traced to the different effects of quantum interference on coherent population trapping (CPT). For the V atom, quantum interference and coherent excitation combine to lead to CPT. For the A atom, however, the quantum interference tends to spoil CPT while the coherent excitation induces the effect.

  13. Atomic phase diagram

    Institute of Scientific and Technical Information of China (English)

    LI Shichun

    2004-01-01

    Based on the Thomas-Fermi-Dirac-Cheng model, atomic phase diagram or electron density versus atomic radius diagram describing the interaction properties of atoms of different kinds in equilibrium state is developed. Atomic phase diagram is established based on the two-atoms model. Besides atomic radius, electron density and continuity condition for electron density on interfaces between atoms, the lever law of atomic phase diagram involving other physical parameters is taken into account, such as the binding energy, for the sake of simplicity.

  14. PT-GC-CAFS联用技术测定污水处理厂外排水中烷基汞残留量%Determination of the Alkyl Mercury Residue in External Drainage of Partial of Sewage Treatment Plants by Purging Capture-Gas Chromatography-Cold Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    高兰兰; 徐浩; 杨琼; 戴刚

    2016-01-01

    建立了吹扫捕集-气相色谱-冷原子荧光( PT-GC-CAFS)联用技术、多功能自动进样器进样测定污水处理厂外排水中烷基汞残留量的方法. 用烷基化试剂直接衍生,吹扫捕集吸附/富集,以PEG20M填充柱为分离柱,用冷原子荧光作为检测器进行测定,整体分析工作在10 min内完成. 在所选实验条件下,方法对所测甲基汞、乙基汞的线性相关系数分别为0.999 9、1.000,最低检出限分别为0.002、0.003 ng/L,相对标准偏差为1.4% ~10.2%,2.3% ~9.7%;在不同质量浓度水平上进行加标回收率实验,甲基汞的回收率为93.7% ~101.7%,乙基汞为94.1% ~103.6%. 该方法用于污水处理厂外排水中烷基汞残留量的分析测定,结果令人满意.%A confirmative method was developed with purge and trap-GC separation-cold atomic fluorescence spectrophotometer ( PT-GC-CAFS) to detect the residues of alkyl mercury in external drainage of sewage treatment plants by multifunctional automatic sampler. Using direct derivative alkyl mercury by Alkylating reagent, adsorption/enrichment by PT, with PEG20M packed column for separation column, and with cold atomic fluorescence spectrophotometer as a detector to detect mercury in environmental water samples, the overall analysis of the work to be done within 10 min. The method showed that good linear correlation coefficient of methyl mercury′s and ethyl mercury′s was 0.999 9 and 1.000, the relative standard deviation was (RSD=1.4%-10.2%) and ( RSD=2.3%-9.7%) , respectively. With different quality levels to Standard addition recovery test sample, the recovery rate of methyl mercury was 93.7%-101.7%, ethyl mercury was 94.1%-103.6%. The method was applied to determine the alkyl mercury residue in external drainage samples of sewage treatment plants. The results were satisfactory.

  15. Determination of As,Hg and Cd in FAPAS Canned Fish in UK by Hydride Generation-Atomic Fluorescence Spectrometry%氢化物-原子荧光光谱法测定英国FAPAS鱼罐头中砷汞镉

    Institute of Scientific and Technical Information of China (English)

    叶海辉; 谢德芳; 谢轶; 吴学进

    2012-01-01

    [Objective] To prove that the determination of As, Hg and Cd by the hydride generation-atomic fluorescence spectrometry (HG-AFS) has reached the international level of advanced detection instrument. [ Method] The parameters and testing methods of the HG-AFS were optimized. Through the testing of samples and the recovery test, a set of methods were established for determining the three elements in FAPAS canned fish. [Result] By comparing the detection report provided by FAPAS with the results of multiple laboratories, the Z value was -0.2 for As, 0. 5 for Hg, and 0.4 for Cd, the evaluation of results was satisfactory. [ Conclusion] It is feasible'to apply the HG-AFS method for the determination of As, Hg and Cd in seafood products.%[目的]证实原子荧光仪对这砷汞镉3种元素的检测已达到国际先进检测仪器的水平.[方法]利用氢化物-原子荧光光谱法,优化仪器条件参数和试验方法,通过测试质控样品与加标回收试验,建立一套测试英国FAPAS鱼罐头中砷汞镉的方法.[结果]根据FAPAS提供回来的检测报告,与全球众多实验室比对的结果为:砷的Z值为-0.2,汞的Z值为0.5,镉的Z值为0.4,对结果的评价为很满意.[结论]应用氢化物-原子荧光光谱法对海产品中砷汞镉进行检测是可行的.

  16. 微波消解-氢化物原子荧光光谱法测定粤东地区海产品中砷的研究%Determination of Arsenic in Seafood by Hydride Generation-atomic Fluorescence Spectrometry Combined with Microwave Oven Digestion

    Institute of Scientific and Technical Information of China (English)

    蔡龙飞; 徐春秀; 张应钦; 邱新红

    2011-01-01

    [目的]建立一种测定海产品中微量砷的有效方法.[方法]采用微波消解-氢化物原子荧光光谱法测定了粤东地区海产品中砷的含量.[结果]砷在1.0~50.0μg/L范围内线性关系良好,相关系数为0.995,方法的检出限为0.02107μg/L,相对标准偏差为0.932%.部分海产品的含砷量超过国家标准,其超标原因可能与沿海地区的工业污染有关.[结论]该方法试剂用量少、污染小、简便、快速、准确,适于各类海产品中砷含量的检测.%[Objective] The aim was to establish an effective determination method of arsenic in seafood. [Method] Contents of arsenic in seafood samples from eastern Guangdong area were determined by hydride generation-atomic fluorescence spectrometry combined with microwave oven digestion. [Result] The linear range for detection of arsenic was 1.0- 50.0 μg/L, which showed a good linear relationship,and its correlation coefficient was 0.995. The detection limit and relative standard deviation were 0.021 07 μg/L and 0.932% .respectively. Contents of arsenic in some seafood samples were more than the national standard,which could be caused by industrial pollution in coastal areas. [Conclusion] The method is simple,rapid and accurate,so it is applied to the determination of arsenic in seafood samples.

  17. Cold Matter Assembled Atom-by-Atom

    CERN Document Server

    Endres, Manuel; Keesling, Alexander; Levine, Harry; Anschuetz, Eric R; Krajenbrink, Alexandre; Senko, Crystal; Vuletic, Vladan; Greiner, Markus; Lukin, Mikhail D

    2016-01-01

    The realization of large-scale fully controllable quantum systems is an exciting frontier in modern physical science. We use atom-by-atom assembly to implement a novel platform for the deterministic preparation of regular arrays of individually controlled cold atoms. In our approach, a measurement and feedback procedure eliminates the entropy associated with probabilistic trap occupation and results in defect-free arrays of over 50 atoms in less than 400 ms. The technique is based on fast, real-time control of 100 optical tweezers, which we use to arrange atoms in desired geometric patterns and to maintain these configurations by replacing lost atoms with surplus atoms from a reservoir. This bottom-up approach enables controlled engineering of scalable many-body systems for quantum information processing, quantum simulations, and precision measurements.

  18. Fluorescence antibunching microscopy

    CERN Document Server

    Schwartz, Osip

    2011-01-01

    Breaking the diffraction limit in microscopy by utilizing quantum properties of light has been the goal of intense research in the recent years. We propose a quantum superresolution technique based on non-classical emission statistics of fluorescent markers, routinely used as contrast labels for bio-imaging. The technique can be readily implemented using standard fluorescence microscopy equipment.

  19. LEDs for fluorescence microscopy

    NARCIS (Netherlands)

    Young, I.T.; Garini, Y.; Dietrich, H.R.C.; Van Oel, W.; Liqui Lung, G.

    2004-01-01

    Traditional light sources for fluorescence microscopy have been mercury lamps, xenon lamps, and lasers. These sources have been essential in the development of fluorescence microscopy but each can have serious disadvantages: lack of near monochromaticity, heat generation, cost, lifetime of the light

  20. Fluorescence of atopic allergens

    NARCIS (Netherlands)

    Berrens, L.

    1967-01-01

    Purified atopic allergens have been found to emit flue fluorescence upon irradiation with ultraviolet light of 365 mμ wavelength. The maximum of fluorescence is in the region 445–490 mμ and the intensity is of the same order of magnitude for different atopic allergens. Synthetic model compounds, inc

  1. Different Algorithms for Improving Detection Power of Atomic Fluorescence Spectrometry

    Directory of Open Access Journals (Sweden)

    Jian Cui

    2012-11-01

    Full Text Available The purpose of detecting trace concentrations of analytes often is hindered by occurring noise in the signal curves of analytical methods. This is also a problem when different arsenic species (organic arsenic species such as arsanilic acid, nitarsone and roxarsone are to be determined in animal meat by HPLC-UV-HG-AFS, which is the basis of this work. In order to improve the detection power, methods of signal treatment may be applied. We show a comparison of convolution with Gaussian distribution curves, Fourier transform, and wavelet transform. It is illustrated how to estimate decisive parameters for these techniques. All methods result in improved limits of detection. Furthermore, applying baselines and evaluating peaks thoroughly is facilitated. However, there are differences. Fourier transform may be applied, but convolution with Gaussian distribution curves shows better results of improvement. The best of the three is wavelet transform, whereby the detection power is improved by factors of about 2.4

  2. Atomic hydrogen behaviour in Heliotron E

    Energy Technology Data Exchange (ETDEWEB)

    Muraoka, K.; Uchino, K.; Kajiwara, T.; Matsuo, K.; Honda, C.; Suehiro, Y.; Yano, N.; Takeda, K.; Hagiwara, H.; Akazaki, M. (Kyushu Univ., Fukuoka (Japan). Dept. of Energy Conversion); Maeda, M.; Okada, T. (Kyushu Univ., Fukuoka (Japan). Dept. of Electrical Engineering); Sudo, S.; Kondo, K.; Mizuuchi, T.; Sano, F.; Sato, M.; Zushi, H.; Obiki, T. (Kyoto Univ., Uji (Japan). Plasma Physics Lab.); Matsuura, H. (Osaka Prefectural Univ., Sakai (Japan). Dept. of Mechanical Engineering)

    1990-12-01

    In order to understand atomic hydrogen behaviour and particle confinement properties in Heliotron E plasmas, techniques of laser induced fluorescence (LIF) have been extensively used, combined with measurements of absolute Balmer alpha emissions and density fluctuations. The results revealed that for an average electron density anti n{sub e}>1.5x10{sup 19} m{sup -3}, H{alpha} fluorescence allowed the measurements of atomic hydrogen densities and yielded the recycled Franck-Condon neutrals ({approx equal} 3 eV) to penetrate into core plasmas, whereas for anti n{sub e}<1.0x10{sup 19} m{sup -3}, such measurements were perturbed by dissociative-excitation of H{sub 2} molecules into the n=2 state. Also, the global confinement times showed a clear correlation with electron density fluctuations. (orig.).

  3. Single Molecule DNA Detection with an Atomic Vapor Notch Filter

    CERN Document Server

    Uhland, Denis; Widmann, Matthias; Lee, Sang-Yun; Wrachtrup, Jörg; Gerhardt, Ilja

    2015-01-01

    The detection of single molecules has facilitated many advances in life- and material-sciences. Commonly, it founds on the fluorescence detection of single molecules, which are for example attached to the structures under study. For fluorescence microscopy and sensing the crucial parameters are the collection and detection efficiency, such that photons can be discriminated with low background from a labeled sample. Here we show a scheme for filtering the excitation light in the optical detection of single stranded labeled DNA molecules. We use the narrow-band filtering properties of a hot atomic vapor to filter the excitation light from the emitted fluorescence of a single emitter. The choice of atomic sodium allows for the use of fluorescent dyes, which are common in life-science. This scheme enables efficient photon detection, and a statistical analysis proves an enhancement of the optical signal of more than 15% in a confocal and in a wide-field configuration.

  4. 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.

  5. Malevolent use of radioactive materials: An international exercise in the analysis of gamma-spectrometric data

    DEFF Research Database (Denmark)

    Dowdall, M.; Andersson, Kasper Grann; Palsson, S.E.

    2010-01-01

    with isotopes and activities that present significant challenges with respect to identification and quantification using gamma ray spectrometry. The MALRAD international exercise was designed to provide a practice opportunity for authorities and laboratories to work with synthetic gamma-spectrometric data...... isotopes, irrespective of the detector type involved, all participants were in a position to identify sources and provide estimates of activity. For situations involving shielded sources or special nuclear materials most participants were in a position to provide indications as to what the sources were...

  6. Electron Ionization Mass Spectrometric Study of Some Substituted 1,3-oxazoles

    OpenAIRE

    Salgueiro, Pedro; Dias, Catarina; Carreiras, M. Carmo; Borges, Carlos

    2007-01-01

    Comunicação oral sob a forma painel Heterocyclic compounds are widely used as pharmaceuticals. Tacrine (THA) was the first drug approved for the treatment of Alzheimer’s disease (AD) and a great effort has been made to design and synthesize new THA-analogues in order to evaluate their beneficial effects as therapeutic agents in this disease.1-6 Contrasting with the pharmaceutical interest, mass spectrometric studies of these compounds and of some of its precursors, namely the oxazole and o...

  7. Tandem mass spectrometric fragmentation patterns of known and new steviol glycosides with structure proposals.

    Science.gov (United States)

    Zimmermann, Benno F

    2011-06-15

    Stevia rebaudiana contains several steviol glycosides that have a sweet flavor. They are up to 450 times sweeter than sucrose, but some have an undesirable aftertaste. Up to 2010, ten different steviol glycosides have been described from the leaves or purified extracts of S. rebaudiana. In this paper, the tandem mass spectrometric fragmentation patterns of these ten compounds are compiled, along with a scheme for structural elucidation. This scheme is then applied to 12 steviol glycosides that have not yet been described. The proposed structures of five steviol glycosides have been confirmed by other authors.

  8. Fluorescence and Spectral Imaging

    Directory of Open Access Journals (Sweden)

    Ralph S. DaCosta

    2007-01-01

    Full Text Available Early identification of dysplasia remains a critical goal for diagnostic endoscopy since early discovery directly improves patient survival because it allows endoscopic or surgical intervention with disease localized without lymph node involvement. Clinical studies have successfully used tissue autofluorescence with conventional white light endoscopy and biopsy for detecting adenomatous colonic polyps, differentiating benign hyperplastic from adenomas with acceptable sensitivity and specificity. In Barrett's esophagus, the detection of dysplasia remains problematic because of background inflammation, whereas in the squamous esophagus, autofluorescence imaging appears to be more dependable. Point fluorescence spectroscopy, although playing a crucial role in the pioneering mechanistic development of fluorescence endoscopic imaging, does not seem to have a current function in endoscopy because of its nontargeted sampling and suboptimal sensitivity and specificity. Other point spectroscopic modalities, such as Raman spectroscopy and elastic light scattering, continue to be evaluated in clinical studies, but still suffer the significant disadvantages of being random and nonimaging. A recent addition to the fluorescence endoscopic imaging arsenal is the use of confocal fluorescence endomicroscopy, which provides real-time optical biopsy for the first time. To improve detection of dysplasia in the gastrointestinal tract, a new and exciting development has been the use of exogenous fluorescence contrast probes that specifically target a variety of disease-related cellular biomarkers using conventional fluorescent dyes and novel potent fluorescent nanocrystals (i.e., quantum dots. This is an area of great promise, but still in its infancy, and preclinical studies are currently under way.

  9. Hyperfine Magnetic Anomaly in the Atomic Spectra of the Rare-Earth Elements

    CERN Document Server

    Gangrsky, Yu P; Karaivanov, D V; Kolesnikov, N N; Marinova, K P; Markov, B N; Rostovsky, V S

    2001-01-01

    The constants of the hyperfine splitting in the atomic optical spectra of the rare-earth elements - Nd, Eu, Gd and Lu - were measured. The method of laser resonance fluorescence in the parallel atomic beam was used. The values of the hyperfine magnetic anomaly were determined from the comparison of magnetic dipole constant ratios of the neighbouring odd Z or N isotopes for the different atomic levels. The connection of these values and the parameters of atomic and nuclear structure is discussed.

  10. MALDI-mass spectrometric imaging revealing hypoxia-driven lipids and proteins in a breast tumor model

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Jiang; Chughtai, Kamila; Purvine, Samuel O.; Bhujwalla, Zaver M.; Raman, Venu; Pasa-Tolic, Ljiljana; Heeren, Ronald M.; Glunde, Kristine

    2015-06-16

    Hypoxic areas are a common feature of rapidly growing malignant tumors and their metastases, and are typically spatially heterogeneous. Hypoxia has a strong impact on tumor cell biology and contributes to tumor progression in multiple ways. To date, only a few molecular key players in tumor hypoxia, such as for example hypoxia-inducible factor-1 (HIF-1), have been discovered. The distribution of biomolecules is frequently heterogeneous in the tumor volume, and may be driven by hypoxia and HIF-1α. Understanding the spatially heterogeneous hypoxic response of tumors is critical. Mass spectrometric imaging (MSI) provides a unique way of imaging biomolecular distributions in tissue sections with high spectral and spatial resolution. In this paper, breast tumor xenografts grown from MDA-MB-231-HRE-tdTomato cells, with a red fluorescent tdTomato protein construct under the control of a hypoxia response element (HRE)-containing promoter driven by HIF-1α, were used to detect the spatial distribution of hypoxic regions. We elucidated the 3D spatial relationship between hypoxic regions and the localization of small molecules, metabolites, lipids, and proteins by using principal component analysis – linear discriminant analysis (PCA-LDA) on 3D rendered MSI volume data from MDA-MB-231-HRE-tdTomato breast tumor xenografts. In this study we identified hypoxia-regulated proteins active in several distinct pathways such as glucose metabolism, regulation of actin cytoskeleton, protein folding, translation/ribosome, splicesome, the PI3K-Akt signaling pathway, hemoglobin chaperone, protein processing in endoplasmic reticulum, detoxification of reactive oxygen species, aurora B signaling/apoptotic execution phase, the RAS signaling pathway, the FAS signaling pathway/caspase cascade in apoptosis and telomere stress induced senescence. In parallel we also identified co-localization of hypoxic regions and various lipid species such as PC(16:0/18:1), PC(16:0/18:2), PC(18:0/18:1), PC

  11. Atom Lithography with a Chromium Atomic Beam

    Institute of Scientific and Technical Information of China (English)

    ZHANG Wen-Tao; LI Tong-Bao

    2006-01-01

    @@ Direct write atom lithography is a new technique in which resonant light is used to pattern an atomic beam and the nanostructures are formed when the atoms deposit on the substrate. We design an experiment setup to fabricate chromium nanolines by depositing an atomic beam of 52 Cr through an off-resonant laser standing wave with the wavelength of 425.55 nm onto a silicon substrate. The resulting nanolines exhibit a period of 215 ± 3 nm with height of 1 nm.

  12. Highly thermostable fluorescent proteins

    Science.gov (United States)

    Bradbury, Andrew M.; Waldo, Geoffrey S.; Kiss, Csaba

    2011-03-22

    Thermostable fluorescent proteins (TSFPs), methods for generating these and other stability-enhanced proteins, polynucleotides encoding such proteins, and assays and method for using the TSFPs and TSFP-encoding nucleic acid molecules are provided. The TSFPs of the invention show extremely enhanced levels of stability and thermotolerance. In one case, for example, a TSFP of the invention is so stable it can be heated to 99.degree. C. for short periods of time without denaturing, and retains 85% of its fluorescence when heated to 80.degree. C. for several minutes. The invention also provides a method for generating stability-enhanced variants of a protein, including but not limited to fluorescent proteins.

  13. Measurement of visible and UV emission from Energetic Neutral Atom Precipitation (ENAP), on Spacelab

    Science.gov (United States)

    Tinsley, B. A.

    1980-01-01

    The charge exchange of plasmaspheric ions and exospheric H and O and of solar wind ions with exospheric and interplanetary H are sources of precipitating neutrals whose faint emission may be observed by the imaging spectrometric observatory during dark periods of the SL-1 orbit. Measurements of the interactions of these precipitating atoms with the thermosphere are needed to evaluate the heating and ionization effects on the atmosphere as well as the selective loss of i energetic ions from the sources (predominantly the ring current).

  14. Cooperative effects and slow dynamics of fluorescence intensity from quantum emitters in a dielectric

    Science.gov (United States)

    Lozing, N. A.; Gladush, M. G.

    2016-12-01

    We study theoretically the possibility of spontaneous switching between dim and bright fluorescence modes from a cooperative ensemble of two-level atoms driven by a cw-laser. A numerical analysis of transient regimes and transformations of the fluorescence spectrum are reported.

  15. Mass spectrometric studies of cis- and trans-1a,3-disubstituted-1,1-dichloro-4-formyl-1a, 2,3,4-tetrahydro-1H-azirino [ 1,2-a ][ 1,5 ] benzodiazepines

    Institute of Scientific and Technical Information of China (English)

    XU, Jia-Xi(许家喜); ZHANG, Xin-Yu(张新宇); JIN, Sheng(金声)

    2000-01-01

    The mass spectrometric behaviour of four cis- and trans-1a,3- disubstituted -1,1 - dichloro-4-formyl-1a,2,3,4-tetrahydro1H-azirino[1,2-a] [1,5] benzodiazepines has been studied with the aid of mass-analysed ion kinetic energy spectrometry and exact mass measurements under electron impact ionization. All compounds show a tendency to eliminate a chlorine atom from the aziridine ring, and then eliminate a neutral propene or styrene from the diazepine ring to yield azirino[1,2-b][1,3]benzimidazole ions. These azirino[1,2-a] [1,5]-benzodiazepines can also eliminate HCl, or Cl plus HCl simultaneously to undergo a ring enlargement rearrangement to yield 1,6-benzodiazocine ions, which further lose small molecular fragments, propyne or phenylacetylene, with rearrangement to give quinoxaline ions.

  16. Advances in atomic spectroscopy

    CERN Document Server

    Sneddon, J

    2000-01-01

    This fifth volume of the successful series Advances in Atomic Spectroscopy continues to discuss and investigate the area of atomic spectroscopy.It begins with a description of the use of various atomic spectroscopic methods and applications of speciation studies in atomic spectroscopy. The emphasis is on combining atomic spectroscopy with gas and liquid chromatography. In chapter two the authors describe new developments in tunable lasers and the impact they will have on atomic spectroscopy. The traditional methods of detection, such as photography and the photomultiplier, and how they are being replaced by new detectors is discussed in chapter three. The very active area of glow discharge atomic spectrometry is presented in chapter four where, after a brief introduction and historical review, the use of glow discharge lamps for atomic spectroscopy and mass spectrometry are discussed. Included in this discussion is geometry and radiofrequency power. The future of this source in atomic spectroscopy is also dis...

  17. Atomic and molecular manipulation

    CERN Document Server

    Mayne, Andrew J

    2011-01-01

    Work with individual atoms and molecules aims to demonstrate that miniaturized electronic, optical, magnetic, and mechanical devices can operate ultimately even at the level of a single atom or molecule. As such, atomic and molecular manipulation has played an emblematic role in the development of the field of nanoscience. New methods based on the use of the scanning tunnelling microscope (STM) have been developed to characterize and manipulate all the degrees of freedom of individual atoms and molecules with an unprecedented precision. In the meantime, new concepts have emerged to design molecules and substrates having specific optical, mechanical and electronic functions, thus opening the way to the fabrication of real nano-machines. Manipulation of individual atoms and molecules has also opened up completely new areas of research and knowledge, raising fundamental questions of "Optics at the atomic scale", "Mechanics at the atomic scale", Electronics at the atomic scale", "Quantum physics at the atomic sca...

  18. 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.

  19. Time-resolved visible/near-infrared spectrometric observations of the Galaxy 11 geostationary satellite

    Science.gov (United States)

    Bédard, Donald; Wade, Gregg A.

    2017-01-01

    Time-resolved spectrometric measurements of the Galaxy 11 geostationary satellite were collected on three consecutive nights in July 2014 with the 1.6-m telescope at the Observatoire du Mont-Mégantic in Québec, Canada. Approximately 300 low-resolution spectra (R ≈ 700 , where R = λ / Δλ) of the satellite were collected each night, covering a spectral range between 425 and 850 nm. The two objectives of the experiment were to conduct material-type identification from the spectra and to study how the spectral energy distribution inferred from these measurements varied as the illumination and observation geometry changed on nightly timescales. We present results that indicate the presence of a highly reflective aluminized surface corresponding to the solar concentrator arrays of the Galaxy 11 spacecraft. Although other material types could not be identified using the spectra, the results showed that the spectral energy distribution of the reflected sunlight from the Galaxy 11 spacecraft varied significantly, in a systematic manner, over each night of observation. The variations were quantified using colour indices calculated from the time-resolved spectrometric measurements.

  20. Ambient aerodynamic ionization source for remote analyte sampling and mass spectrometric analysis.

    Science.gov (United States)

    Dixon, R Brent; Sampson, Jason S; Hawkridge, Adam M; Muddiman, David C

    2008-07-01

    The use of aerodynamic devices in ambient ionization source development has become increasingly prevalent in the field of mass spectrometry. In this study, an air ejector has been constructed from inexpensive, commercially available components to incorporate an electrospray ionization emitter within the exhaust jet of the device. This novel aerodynamic device, herein termed remote analyte sampling, transport, and ionization relay (RASTIR) was used to remotely sample neutral species in the ambient and entrain them into an electrospray plume where they were subsequently ionized and detected using a linear ion trap Fourier transform mass spectrometer. Two sets of experiments were performed in the ambient environment to demonstrate the device's utility. The first involved the remote (approximately 1 ft) vacuum collection of pure sample particulates (i.e., dry powder) from a glass slide, entrainment and ionization at the ESI emitter, and mass spectrometric detection. The second experiment involved the capture (vacuum collection) of matrix-assisted laser desorbed proteins followed by entrainment in the ESI emitter plume, multiple charging, and mass spectrometric detection. This approach is in principle a RASTIR-assisted matrix-assisted laser desorption electrospray ionization source (Sampson, J. S.; Hawkridge, A. M.; Muddiman, D. C. J. Am. Soc. Mass Spectrom. 2006, 17, 1712-1716; Rapid Commun. Mass Spectrom. 2007, 21, 1150-1154.). A detailed description of the device construction, operational parameters, and preliminary small molecule and protein data are presented.

  1. 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.

  2. The role of peroxyl radicals in polyester degradation--a mass spectrometric product and kinetic study using the distonic radical ion approach.

    Science.gov (United States)

    Gervasoni, B D; Khairallah, G N; O'Hair, R A J; Wille, U

    2015-04-14

    Mass spectrometric techniques were used to obtain detailed insight into the reactions of peroxyl radicals with model systems of (damaged) polyesters. Using a distonic radical ion approach, it was shown that N-methylpyridinium peroxyl radical cations, Pyr(+)OO˙, do not react with non-activated C-H bonds typically present in polyesters that resist degradation. Structural damage in the polymer, for example small amounts of alkene moieties formed during the manufacturing process, is required to enable reaction with Pyr(+)OO˙, which proceeds with high preference through addition to the π system rather than via allylic hydrogen atom abstraction (kadd/kHAT > 20 for internal alkenes). This is due to the very fast and strongly exothermic subsequent fragmentation of the peroxyl-alkene radical adduct to epoxides and highly reactive Pyr(+)O˙, which both could promote further degradation of the polymer through non-radical and radical pathways. This work provides essential experimental support that the basic autoxidation mechanism is a too simplistic model to rationalize radical mediated degradation of polymers under ambient conditions.

  3. Purge and Trap Gas Chromatography-Cold Vapor Atomic Fluorescence Spectrometry Determination of Methyl Mercury and Ethyl Mercury in Marine Animals%P & T-GC-CVAFS法测定海产动物中的甲基汞和乙基汞

    Institute of Scientific and Technical Information of China (English)

    崔颖; 肖亚兵; 王禹; 高健会

    2016-01-01

    Marine animals sample was extracted with 30%nitric acid solution , and then adjusted the pH with 2 mol/L sodium acetate-acetic acid buffer solution. The eluate obtained was determined and identified by purge and trap gas chromatography-cold vapor atomic fluorescence spectrometry (P&T-GC-CVAFS). The propylation derivatization converted Methyl mercury (MeHg) to the more volatile methyl propyl mercury (MeHgPr), Ethyl mercury(EtHg) to the more volatile ethyl propyl mercury(EtHgPr), which could be concentrated through purge and trap system with a further clean-up of matrix. Tests for recovery were made by addition of standard MeHg and EtHg solutions at 3 different concentration levels to blank marine animals sample matrixes, values of MeHg recovery found were in the range from 80.5%to 103.2%, with RSDs (n=6) in the range from 1.7%to 6.9%;values of EtHg recovery found were in the range from 84.2%to 103.7%, with RSDs(n=6) in the range from 2.3%to 7.0%.%海产动物样品经过30%硝酸溶液提取,用2 mol/L醋酸钠-醋酸缓冲溶液调节pH后,用吹扫捕集-气相色谱-冷原子荧光光谱仪联用系统测定其中的甲基汞和乙基汞的含量。使用衍生试剂,将甲基汞转化为甲基丙基汞,乙基汞转化为乙基丙基汞,吹扫捕集进行富集并进一步消除基体干扰。以空白样品为基体,添加3种浓度水平的甲基汞和乙基汞标准溶液,测得甲基汞的回收率为80.5%~103.2%,相对标准偏差(n=6)为1.7%~6.9%;乙基汞的回收率在84.2%~103.7%,相对标准偏差(n=6)为2.3%~7.0%。

  4. 超声波水浴辅助消解-原子荧光光谱法测定食用菌中硒含量%Determination of Selenium in Edible Mushrooms by Ultrasonic Assisted Water Bath Digestion-Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    吴庆晖; 黄伯熹; 冉文清; 荀合; 魏强; 李正全; 陈泳

    2012-01-01

    A method to determine selenium in edible mushroom was developed using ultrasonic assisted water bath digestion followed by atomic fluorescence spectrometry (AFS). The optimum instrumental parameters were established using an orthogonal array design. Besides, the effects of digestion methods and digestion in the presence or absence of potassium ferricyanide on the results of AFS were investigated. AFS was used to determine the selenium contents of different edible mushrooms and the causes of selenium enrichment and the food safety were analyzed based on the results obtained. The limit of detection of the AFS method was 0.20 ng/mL. The sample pretreatment was more efficient and the results of AFS obtained using ultrasonic assisted water bath digestion showed no significant differences compared with wet digestion. AFS can provide a rapid and accurate to analyze selenium in edible mushroom.%为提高检测效率,建立超声波水浴辅助消解.原子荧光光谱法测定食用菌中硒含量的方法。对仪器实验条件进行正交试验优化,对样品前处理方法、铁氰化钾的影响和方法选择性等影响因素进行研究,根据样品检测结果进行原因分析及安全性评价。该方法检出限为0.20ng/mL,加标回收率为91.6%-102.7%。与国标方法对照,提高了样品前处理效率且结果无显著性差异,为食用菌中硒的检测与质量控制提供了一种快速、准确的分析方法。

  5. Simultaneous Determination of Arsenic and Mercury in Compound Danshen Tablets by Double Channel Atomic Fluorescence Spectrometry%双通道原子荧光法同时测定复方丹参片中砷和汞的含量

    Institute of Scientific and Technical Information of China (English)

    莫迎

    2011-01-01

    目的:建立双通道原子荧光法同时测定复方丹参片中砷和汞的含量.方法:样品采用浓硝酸和过氧化氢混合液进行预消化,再采用微波消解仪在3种条件下进行消化.优化的仪器工作参数:光电倍增管负高压为270 V,砷空心阴极灯总电流为60mA,汞空心阴极灯总电流为30 mA,原子化器高度为8 mm,载气流量为400 ml·min-1,屏蔽气流量为800ml·min-1.结果:本方法砷和汞的线性范围分别为0~60ng·ml-1和0~5 ng·ml-1,相关系数分别为r=0.9998(n=6)和r=0.999 5(n=6),检出限分别为1.38μg·kg-1和0.078μg·kg-1,回收率分别为99.34%和98.38%.结论:本法可用于复方丹参片中砷和汞含量的测定.%Objective: To establish a method for the simultaneous determination of arsenic and mercury in compound Danshen tablets by double channel atomic fluorescence spectrometry.Method: The samples were pre-dissolved by nitric acid and hydrogen peroxide, then digested completely using microwave digestion device under 3 different conditions.The measurement conditions were as the follows: the negative high pressure of photomultiplier tubes was 270 v, total current of As hollow cathode lamp was 60 mA and 30 mA for Hg hollow cathode lamp, height of atomizer was 8 mm, carrier gas flow was 400 ml· min -1 and 800 ml· min -1 for shielding gas.Result: The linear range was 0-60 ng·ml-1 and 0-5 ng·ml -1 for arsenic and mercury with the correlation coefficient of 0.999 8( n =6) and 0.9995 ( n = 6 ), respectively.The detection limit of arsenic and mercury was 1.38 μg· kg - 1 and 0.078 μg · kg - 1, and the recovery was 99.34% and 98.38%, respectively.Conclusion: The method can be used for the simultaneous detection of arsenic and mercury in compound Danshen tablets.

  6. Presenting the Bohr Atom.

    Science.gov (United States)

    Haendler, Blanca L.

    1982-01-01

    Discusses the importance of teaching the Bohr atom at both freshman and advanced levels. Focuses on the development of Bohr's ideas, derivation of the energies of the stationary states, and the Bohr atom in the chemistry curriculum. (SK)

  7. Observation of single neutral atoms in a large-magnetic-gradient vapour-cell magneto-optical trap

    Institute of Scientific and Technical Information of China (English)

    Wang Jing; He Jun; Qiu Ying; Yang Bao-Dong; Zhao Jiang-Yan; Zhang Tian-Cai; Wang Jun-Min

    2008-01-01

    Single caesium atoms in a large-magnetic-gradient vapour-cell magneto-optical trap have been identified. The trapping of individual atoms is marked by the steps in fluorescence signal corresponding to the capture or loss of single atoms. The typical magnetic gradient is about 29 mT/cm, which evidently reduces the capture rate of magneto-optical trap.

  8. Atomic Storage States

    Institute of Scientific and Technical Information of China (English)

    汪凯戈; 朱诗尧

    2002-01-01

    We present a complete description of atomic storage states which may appear in the electromagnetically induced transparency (EIT). The result shows that the spatial coherence has been included in the atomic collective operators and the atomic storage states. In some limits, a set of multimode atomic storage states has been established in correspondence with the multimode Fock states of the electromagnetic field. This gives a better understanding of the fact that, in BIT, the optical coherent information can be preserved and recovered.

  9. Atoms Talking to SQUIDs

    CERN Document Server

    Hoffman, J E; Kim, Z; Wood, A K; Anderson, J R; Dragt, A J; Hafezi, M; Lobb, C J; Orozco, L A; Rolston, S L; Taylor, J M; Vlahacos, C P; Wellstood, F C

    2011-01-01

    We present a scheme to couple trapped $^{87}$Rb atoms to a superconducting flux qubit through a magnetic dipole transition. We plan to trap atoms on the evanescent wave outside an ultrathin fiber to bring the atoms to less than 10 $\\mu$m above the surface of the superconductor. This hybrid setup lends itself to probing sources of decoherence in superconducting qubits. Our current plan has the intermediate goal of coupling the atoms to a superconducting LC resonator.

  10. Single Atom Plasmonic Switch

    OpenAIRE

    Emboras, Alexandros; Niegemann, Jens; Ma, Ping; Haffner, Christian; Luisier, Mathieu; Hafner, Christian; Schimmel, Thomas; Leuthold, Juerg

    2015-01-01

    The atom sets an ultimate scaling limit to Moores law in the electronics industry. And while electronics research already explores atomic scales devices, photonics research still deals with devices at the micrometer scale. Here we demonstrate that photonic scaling-similar to electronics-is only limited by the atom. More precisely, we introduce an electrically controlled single atom plasmonic switch. The switch allows for fast and reproducible switching by means of the relocation of an individ...

  11. Atomic Scale Plasmonic Switch

    OpenAIRE

    Emboras, A.; Niegemann, J.; Ma, P.; Haffner, C; Pedersen, A.; Luisier, M.; Hafner, C.; Schimmel, T.; Leuthold, J.

    2016-01-01

    The atom sets an ultimate scaling limit to Moore’s law in the electronics industry. While electronics research already explores atomic scales devices, photonics research still deals with devices at the micrometer scale. Here we demonstrate that photonic scaling, similar to electronics, is only limited by the atom. More precisely, we introduce an electrically controlled plasmonic switch operating at the atomic scale. The switch allows for fast and reproducible switching by means of the relocat...

  12. Identifying tissue-specific signal variation in MALDI mass spectrometric imaging by use of an internal standard

    NARCIS (Netherlands)

    Pirman, D.A.; Kiss, A.; Heeren, R.M.A.; Yost, R.A.

    2013-01-01

    Generating analyte-specific distribution maps of compounds in a tissue sample by matrix-assisted laser desorption/ionization (MALDI) mass spectrometric imaging (MSI) has become a useful tool in numerous areas across the biological sciences. Direct analysis of the tissue sample provides MS images of

  13. Method and apparatus for enhanced sequencing of complex molecules using surface-induced dissociation in conjunction with mass spectrometric analysis

    Science.gov (United States)

    Laskin, Julia [Richland, WA; Futrell, Jean H [Richland, WA

    2008-04-29

    The invention relates to a method and apparatus for enhanced sequencing of complex molecules using surface-induced dissociation (SID) in conjunction with mass spectrometric analysis. Results demonstrate formation of a wide distribution of structure-specific fragments having wide sequence coverage useful for sequencing and identifying the complex molecules.

  14. Atomic Spectra Database (ASD)

    Science.gov (United States)

    SRD 78 NIST Atomic Spectra Database (ASD) (Web, free access)   This database provides access and search capability for NIST critically evaluated data on atomic energy levels, wavelengths, and transition probabilities that are reasonably up-to-date. The NIST Atomic Spectroscopy Data Center has carried out these critical compilations.

  15. Nine New Fluorescent Probes

    Science.gov (United States)

    Lin, Tsung-I.; Jovanovic, Misa V.; Dowben, Robert M.

    1989-06-01

    Absorption and fluorescence spectroscopic studies are reported here for nine new fluorescent probes recently synthesized in our laboratories: four pyrene derivatives with substituents of (i) 1,3-diacetoxy-6,8-dichlorosulfonyl, (ii) 1,3-dihydroxy-6,8-disodiumsulfonate, (iii) 1,3-disodiumsulfonate, and (iv) l-ethoxy-3,6,8-trisodiumsulfonate groups, and five [7-julolidino] coumarin derivatives with substituents of (v) 3-carboxylate-4-methyl, (vi) 3- methylcarboxylate, (vii) 3-acetate-4-methyl, (viii) 3-propionate-4-methyl, and (ix) 3-sulfonate-4-methyl groups. Pyrene compounds i and ii and coumarin compounds v and vi exhibit interesting absorbance and fluorescence properties: their absorption maxima are red shifted compared to the parent compound to the blue-green region, and the band width broadens considerably. All four blue-absorbing dyes fluoresce intensely in the green region, and the two pyrene compounds emit at such long wavelengths without formation of excimers. The fluorescence properties of these compounds are quite environment-sensitive: considerable spectral shifts and fluorescence intensity changes have been observed in the pH range from 3 to 10 and in a wide variety of polar and hydrophobic solvents with vastly different dielectric constants. The high extinction and fluorescence quantum yield of these probes make them ideal fluorescent labeling reagents for proteins, antibodies, nucleic acids, and cellular organelles. The pH and hydrophobicity-dependent fluorescence changes can be utilized as optical pH and/or hydrophobicity indicators for mapping environmental difference in various cellular components in a single cell. Since all nine probes absorb in the UV, but emit at different wavelengths in the visible, these two groups of compounds offer an advantage of utilizing a single monochromatic light source (e.g., a nitrogen laser) to achieve multi-wavelength detection for flow cytometry application. As a first step to explore potential application in

  16. Stroboscopic fluorescence lifetime imaging.

    Science.gov (United States)

    Holton, Mark D; Silvestre, Oscar R; Errington, Rachel J; Smith, Paul J; Matthews, Daniel R; Rees, Paul; Summers, Huw D

    2009-03-30

    We report a fluorescence lifetime imaging technique that uses the time integrated response to a periodic optical excitation, eliminating the need for time resolution in detection. A Dirac pulse train of variable period is used to probe the frequency response of the total fluorescence per pulse leading to a frequency roll-off that is dependent on the relaxation rate of the fluorophores. The technique is validated by demonstrating wide-field, realtime, lifetime imaging of the endocytosis of inorganic quantum dots by a cancer cell line. Surface charging of the dots in the intra-cellular environment produces a switch in the fluorescence lifetime from approximately 40 ns to technique offers lifetime based imaging at video rates with standard CCD cameras and has application in probing millisecond cell dynamics and in high throughput imaging assays.

  17. Single Atom Plasmonic Switch

    CERN Document Server

    Emboras, Alexandros; Ma, Ping; Haffner, Christian; Luisier, Mathieu; Hafner, Christian; Schimmel, Thomas; Leuthold, Juerg

    2015-01-01

    The atom sets an ultimate scaling limit to Moores law in the electronics industry. And while electronics research already explores atomic scales devices, photonics research still deals with devices at the micrometer scale. Here we demonstrate that photonic scaling-similar to electronics-is only limited by the atom. More precisely, we introduce an electrically controlled single atom plasmonic switch. The switch allows for fast and reproducible switching by means of the relocation of an individual or at most - a few atoms in a plasmonic cavity. Depending on the location of the atom either of two distinct plasmonic cavity resonance states are supported. Experimental results show reversible digital optical switching with an extinction ration of 10 dB and operation at room temperature with femtojoule (fJ) power consumption for a single switch operation. This demonstration of a CMOS compatible, integrated quantum device allowing to control photons at the single-atom level opens intriguing perspectives for a fully i...

  18. Condensed matter applied atomic collision physics, v.4

    CERN Document Server

    Datz, Sheldon

    1983-01-01

    Applied Atomic Collision Physics, Volume 4: Condensed Matter deals with the fundamental knowledge of collision processes in condensed media.The book focuses on the range of applications of atomic collisions in condensed matter, extending from effects on biological systems to the characterization and modification of solids. This volume begins with the description of some aspects of the physics involved in the production of ion beams. The radiation effects in biological and chemical systems, ion scattering and atomic diffraction, x-ray fluorescence analysis, and photoelectron and Auger spectrosc

  19. 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.

  20. XRD Analysis on the Fluorescence Material of Sm Doped Si-Ca-Mg System

    Institute of Scientific and Technical Information of China (English)

    HUANG Qing-Ming

    2007-01-01

    Fluorescence material of Sm doped Si-Ca-Mg system was synthesized by using the method of solid phase reaction at high temperature. The phase composition and crystal structure of this material were analyzed with XRD method for its composition and the existence form of Sm atom. We aimed to exactly determine the phase composition of this fluorescence material and the doping position and environment of rare-earth Sm atom in the system because these factors have significant effects on the properties. The analytical results show that the Sm atoms dope in Ca2O26Si6Sm8 lattice in the form of atomic site-occupation in three different space positions with different occupancy rates. Therefore, based on the XRD analytical results, the fluorescence material of Sm doped Si-Ca-Mg system with high performance can be synthesized.

  1. 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.

  2. Gas chromatography-mass spectrometric method for metabolic profiling of tobacco leaves.

    Science.gov (United States)

    Li, Yong; Pang, Tao; Li, Yanli; Wang, Xiaolin; Li, Qinghua; Lu, Xin; Xu, Guowang

    2011-06-01

    A gas chromatography-mass spectrometric method was developed for profiling of tobacco leaves. The differentiation among tobacco leaves planted in two different regions was investigated. Prior to analysis, the extraction solvent formulation was optimized and a combination of water, methanol and acetonitrile with a volume ratio of 3:1:1 was found to be optimal. The reproducibility of the method was satisfactory. Kendall tau-b rank correlation coefficients were equal to 1 (pleaves from Zimbabwe and Yunnan of China. Our result revealed that levels of saccharides and their derivatives including xylose, ribose, fructose, glucose, turanose, xylitol and glyceric acid were more abundant while sucrose, glucitol and D-gluconic acid were less abundant in tobacco leaves from Yunnan as compared to those from Zimbabwe. Amino acids such as L-alanine, L-tyrosine and L-threonine were found to be richer in Zimbabwe tobacco than in Yunnan tobacco.

  3. Considerations for quantification of lipids in nerve tissue using MALDI mass spectrometric imaging

    Science.gov (United States)

    Landgraf, Rachelle R.; Garrett, Timothy J.; Prieto Conaway, Maria C.; Calcutt, Nigel A.; Stacpoole, Peter W.; Yost, Richard A.

    2013-01-01

    MALDI mass spectrometric imaging is a technique that provides the ability to identify and characterize endogenous and exogenous compounds spatially within tissue with relatively little sample preparation. While it is a proven methodology for qualitative analysis, little has been reported for its utility in quantitative measurements. In the current work, inherent challenges in MALDI quantification are addressed. Signal response is monitored over successive analyses of a single tissue section to minimize error due to variability in the laser, matrix application, and sample inhomogeneity. Methods for the application of an internal standard to tissue sections are evaluated and used to quantify endogenous lipids in nerve tissue. A precision of 5% or less standard error was achieved, illustrating that MALDI imaging offers a reliable means of in situ quantification for microgram-sized samples and requires minimal sample preparation. PMID:21953974

  4. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  5. A superheterodyne spectrometer for electronic paramagnetic. Resonance; Spectrometre superheterodyne de resonance paramagnetique electronique

    Energy Technology Data Exchange (ETDEWEB)

    Laffon, J.L. [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1963-12-15

    After a few generalities about electron paramagnetic resonance, a consideration of different experimental techniques authorises the choice of a particular type of apparatus. An EPR superheterodyne spectrometer built in the laboratory and having a novel circuit is described in detail. With this apparatus, many experimental results have been obtained and some of these are described as example. (author) [French] Apres quelques generalites sur le phenomene de resonance paramagnetique electronique, une synthese des differentes techniques experimentales, permet de fixer le choix d'un type d'appareillage. Un spectrometre de RPE superheterodyne realise en laboratoire et comportant un circuit original est expose dans le detail. Cet appareil a permis de nombreux resultats experimentaux dont quelques-uns sont decrits a titre d'exemple. (auteur)

  6. 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.

  7. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 These test methods cover procedures for subsampling and for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of uranium hexafluoride UF6. Most of these test methods are in routine use to determine conformance to UF6 specifications in the Enrichment and Conversion Facilities. 1.2 The analytical procedures in this document appear in the following order: Note 1—Subcommittee C26.05 will confer with C26.02 concerning the renumbered section in Test Methods C761 to determine how concerns with renumbering these sections, as analytical methods are replaced with stand-alone analytical methods, are best addressed in subsequent publications. Sections Subsampling of Uranium Hexafluoride 7 - 10 Gravimetric Determination of Uranium 11 - 19 Titrimetric Determination of Uranium 20 Preparation of High-Purity U3O 8 21 Isotopic Analysis 22 Isotopic Analysis by Double-Standard Mass-Spectrometer Method 23 - 29 Determination of Hydrocarbons, Chlorocarbons, and Partially Substitut...

  8. MASS SPECTROMETRIC ANALYSIS FOR THE IDENTIFICATION OF THUNNUS GENUS FOUR SPECIES

    Directory of Open Access Journals (Sweden)

    T. Pepe

    2011-01-01

    Full Text Available An accurate identification of similar fish species is necessary to prevent illegal substitution and is imposed by labeling regulations in UE countries (1. The genus Thunnus comprises many species of different quality and commercial value. The increasing trade of fish preparations of the species included in this genus and the consequent loss of the external anatomical and morphological features enables fraudulent substitutions. This study reports data relating to the proteomic analysis of four tuna species (T. thynnus, T. alalunga, T. albacares, T. obesus. Sarcoplasmic proteins were studied by mono and two dimensional electrophoresis. The most significant proteins for the characterization of the species were analyzed by mass spectrometric techniques. As reported in a previous study (2, an accurate identification of the species seems possible, owing to the polymorphism displayed by the species of the Thunnus genus.

  9. The 3D inversion of airborne gamma-ray spectrometric data

    Science.gov (United States)

    Minty, Brian; Brodie, Ross

    2016-07-01

    We present a new method for the inversion of airborne gamma-ray spectrometric line data to a regular grid of radioelement concentration estimates on the ground. The method incorporates the height of the aircraft, the 3D terrain within the field of view of the spectrometer, the directional sensitivity of rectangular detectors, and a source model comprising vertical rectangular prisms with the same horizontal dimensions as the required grid cell size. The top of each prism is a plane surface derived from a best-fit plane to the digital elevation model of the earth's surface within each grid cell area. The method is a significant improvement on current methods, and gives superior interpolation between flight lines. It also eliminates terrain effects that would normally remain in the data after the conventional processing of these data assuming a flat-earth model.

  10. Proteogenomics meets cancer immunology: mass spectrometric discovery and analysis of neoantigens.

    Science.gov (United States)

    Polyakova, Anna; Kuznetsova, Ksenia; Moshkovskii, Sergei

    2015-01-01

    Cancer proteogenomics is an emerging field that aims to identify and quantify protein sequence changes associated with the cancer genome. Besides being involved in cancer development and progression, such protein variants may serve as neoantigens, which provide the T-cell response against tumors. Mass spectrometry-based proteogenomics may be a promising tool for finding neoantigens in individual specimens. It is partly based on a technical background accumulated from mass spectrometric studies of peptide ligands of major histocompatibility complex proteins. Examples of the use of mass spectrometry in neoantigen identification are reviewed in this article. Some experimental workflows are discussed, which may use shotgun and targeted proteomics for translational human studies of neoepitopes, such as cancer vaccine development and checkpoint therapy response prediction.

  11. Laser Spectrometric Measurement System for Local Express Diagnostics of Flame at Combustion of Liquid Hydrocarbon Fuels

    Science.gov (United States)

    Kobtsev, V. D.; Kozlov, D. N.; Kostritsa, S. A.; Smirnov, V. V.; Stel'makh, O. M.; Tumanov, A. A.

    2016-03-01

    A laboratory laser spectrometric measurement system for investigation of spatial distributions of local temperatures in a flame at combustion of vapors of various liquid hydrocarbon fuels in oxygen or air at atmospheric pressure is presented. The system incorporates a coherent anti-Stokes Raman spectrometer with high spatial resolution for local thermometry of nitrogen-containing gas mixtures in a single laser shot and a continuous operation burner with a laminar diffusion flame. The system test results are presented for measurements of spatial distributions of local temperatures in various flame zones at combustion of vapor—gas n-decane/nitrogen mixtures in air. Its applicability for accomplishing practical tasks in comparative laboratory investigation of characteristics of various fuels and for research on combustion in turbulent flames is discussed.

  12. Quantitative Mass Spectrometric Analysis and Post-Extraction Stability Assessment of the Euglenoid Toxin Euglenophycin

    Directory of Open Access Journals (Sweden)

    Paul V. Zimba

    2013-09-01

    Full Text Available Euglenophycin is a recently discovered toxin produced by at least one species of euglenoid algae. The toxin has been responsible for several fish mortality events. To facilitate the identification and monitoring of euglenophycin in freshwater ponds, we have developed a specific mass spectrometric method for the identification and quantitation of euglenophycin. The post-extraction stability of the toxin was assessed under various conditions. Euglenophycin was most stable at room temperature. At 8 °C there was a small, but statistically significant, loss in toxin after one day. These methods and knowledge of the toxin’s stability will facilitate identification of the toxin as a causative agent in fish kills and determination of the toxin’s distribution in the organs of exposed fish.

  13. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal compl...... complexes were determined from the ratios of the integrated molecular ion currents of a series of calibration samples containing a porphyrin ester and one of its metal complexes in known molar ratio. Complexes formed with divalent ions of Cu, Zn, Fe, Co and Ni of copro- as well as uro......-prophyrin permethylester were all found to have the same molecular ion sensitivities as their metal-free porphyrin ester. The relative metalloporphyrin ester content in a sample of porphyrin ester was thus obtained directly as the integrated ion current ratios of the normalized molecular ions. The preparation...

  14. Combination of electrochemical, spectrometric and other analytical techniques for high throughput screening of pharmaceutically active compounds.

    Science.gov (United States)

    Suzen, Sibel; Ozkan, Sibel A

    2010-08-01

    Recently, use of electrochemistry and combination of this method with spectroscopic and other analytical techniques are getting one of the important approaches in drug discovery and research as well as quality control, drug stability, determination of physiological activity, measurement of neurotransmitters. Many fundamental physiological processes are depending on oxido-reduction reactions in the body. Therefore, it may be possible to find connections between electrochemical and biochemical reactions concerning electron transfer pathways. Applications of electrochemical techniques to redox-active drug development and studies are one of the recent interests in drug discovery. In this review, the latest developments related to the use of electrochemical techniques in drug research in order to evaluate possible combination spectrometric methods with electrochemical techniques.

  15. 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).

  16. Sublimation as a method of matrix application for mass spectrometric imaging.

    Science.gov (United States)

    Hankin, Joseph A; Barkley, Robert M; Murphy, Robert C

    2007-09-01

    Common organic matrix-assisted laser desorption/ionization (MALDI) matrices, 2,5-dihydroxybenzoic acid, 3,5-dimethoxy-4-hydroxycinnamic acid, and alpha-cyano-4-hydroxycinnamic acid, were found to undergo sublimation without decomposition under conditions of reduced pressure and elevated temperature. This solid to vapor-phase transition was exploited to apply MALDI matrix onto tissue samples over a broad surface in a solvent-free application for mass spectrometric imaging. Sublimation of matrix produced an even layer of small crystals across the sample plate. The deposition was readily controlled with time, temperature, and pressure settings and was highly reproducible from one sample to the next. Mass spectrometric images acquired from phospholipid standards robotically spotted onto a MALDI plate yielded a more intense, even signal with fewer sodium adducts when matrix was applied by sublimation relative to samples where matrix was deposited by an electrospray technique. MALDI matrix could be readily applied to tissue sections on glass slides and stainless steel MALDI plate inserts as long as good thermal contact was made with the condenser of the sublimation device. Sections of mouse brain were coated with matrix applied by sublimation and were imaged using a Q-q-TOF mass spectrometer to yield mass spectral images of very high quality. Image quality is likely enhanced by several features of this technique including the microcrystalline morphology of the deposited matrix, increased purity of deposited matrix, and evenness of deposition. This inexpensive method was reproducible and eliminated the potential for spreading of analytes arising from solvent deposition during matrix application.

  17. GNU polyxmass: a software framework for mass spectrometric simulations of linear (bio-polymeric analytes

    Directory of Open Access Journals (Sweden)

    Rusconi Filippo

    2006-04-01

    Full Text Available Abstract Background Nowadays, a variety of (bio-polymers can be analyzed by mass spectrometry. The detailed interpretation of the spectra requires a huge number of "hypothesis cycles", comprising the following three actions 1 put forth a structural hypothesis, 2 test it, 3 (invalidate it. This time-consuming and painstaking data scrutiny is alleviated by using specialized software tools. However, all the software tools available to date are polymer chemistry-specific. This imposes a heavy overhead to researchers who do mass spectrometry on a variety of (bio-polymers, as each polymer type will require a different software tool to perform data simulations and analyses. We developed a software to address the lack of an integrated software framework able to deal with different polymer chemistries. Results The GNU polyxmass software framework performs common (bio-chemical simulations–along with simultaneous mass spectrometric calculations–for any kind of linear bio-polymeric analyte (DNA, RNA, saccharides or proteins. The framework is organized into three modules, all accessible from one single binary program. The modules let the user to 1 define brand new polymer chemistries, 2 perform quick mass calculations using a desktop calculator paradigm, 3 graphically edit polymer sequences and perform (bio-chemical/mass spectrometric simulations. Any aspect of the mass calculations, polymer chemistry reactions or graphical polymer sequence editing is configurable. Conclusion The scientist who uses mass spectrometry to characterize (bio-polymeric analytes of different chemistries is provided with a single software framework for his data prediction/analysis needs, whatever the polymer chemistry being involved.

  18. Liquid chromatography-mass spectrometric determination of losartan and its active metabolite on dried blood spots.

    Science.gov (United States)

    Rao, R Nageswara; Raju, S Satyanarayana; Vali, R Mastan; Sankar, G Girija

    2012-08-01

    A simple and rapid quantitative bioanalytical liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for simultaneous determination of losartan and its active metabolite, losartan carboxylic acid on rat dried blood spots was developed and validated as per regulatory guidelines. Losartan and its metabolite were extracted from dried blood spots using 50% aqueous methanol and separated on Waters XTerra(®) RP18 (250 mm × 4.6 mm, 5 μm) column using mobile phase composed of 40% acetonitrile and 60% aqueous ammonium acetate (10mM). The eluents were monitored using ESI tandem mass spectrometric detection with negative polarity in MRM mode using ion transitions m/z 421.2→179.0, m/z 435.3→157.0 and m/z 427.3→193.0 for losartan, losartan carboxylic acid and Irbesartan (internal standard), respectively. The method was validated over the linear range of 1-200 ng/mL and 5-1000 ng/mL with lower limits of quantification of 1.0 ng/mL and 5.0 ng/mL for losartan and losartan carboxylic acid, respectively. Inter and intra-day precision and accuracy (Bias) were below 5.96% and between -2.8 and 1.5%, respectively. The mean recoveries of the analytes from dried blood spots were between 89% and 97%. No significant carry over and matrix effects were observed. The stability of stock solution, whole blood, dried blood spot and processed samples were tested under different conditions and the results were found to be well within the acceptable limits. Additional validation parameters such as influence of hematocrit and spot volume were also evaluated and found to be well within the acceptable limits.

  19. 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.

  20. Liquid chromatography-mass spectrometric determination of rufinamide in low volume plasma samples.

    Science.gov (United States)

    Gáll, Zsolt; Vancea, Szende; Dogaru, Maria T; Szilágyi, Tibor

    2013-12-01

    Quantification of rufinamide in plasma was achieved using a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method. The chromatographic separation was achieved on a reversed phase column (Zorbax SB-C18 100mm×3mm, 3.5μm) under isocratic conditions. The mobile phase consisted of a mixture of water containing 0.1% formic acid and methanol (50:50, v/v). The mass spectrometric detection of the analyte was in multiple reaction monitoring mode (MRM) using an electrospray positive ionization (ESI positive). The monitored ions were 127m/z derived from 239m/z rufinamide and 108m/z derived from 251m/z the internal standard (lacosamide). Protein precipitation with methanol was applied for sample preparation using only 50μl aliquots. The concentration range was 40-2000ng/ml for rufinamide in plasma. The limit of detection was 1.25ng/ml and the lower limit of quantification was established at 5ng/ml rufinamide concentration. Selectivity and matrix effect was verified using individual human, rat and rabbit plasma samples. Short-term, post-preparative and freeze-thaw stability was also investigated. The proposed method provides accuracy, precision and high-throughput (short runtime 4.5min) for quantitative determination of rufinamide in plasma. This is the first reported liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for analysis of rufinamide from low volume plasma samples. The LC-MS/MS method was validated according to the current official guidelines and can be applied to accurately measure rufinamide level of large number of plasma samples from clinical studies or therapeutic drug monitoring.

  1. THz Detection and Imaging using Rydberg Atoms

    Science.gov (United States)

    Wade, Christopher; Sibalic, Nikola; Kondo, Jorge; de Melo, Natalia; Adams, Charles; Weatherill, Kevin

    2016-05-01

    Atoms make excellent electromagnetic field sensors because each atom of the same isotope is identical and has well-studied, permanent properties allowing calibration to SI units. Thus far, atoms have not generally been exploited for terahertz detection because transitions from the atomic ground state are constrained to a limited selection of microwave and optical frequencies. In contrast, highly excited `Rydberg' states allow us access to many strong, electric dipole transitions from the RF to THz regimes. Recent advances in the coherent optical detection of Rydberg atoms have been exploited by a number of groups for precision microwave electrometry Here we report the demonstration of a room-temperature, cesium Rydberg gas as a THz to optical interface. We present two configurations: First, THz-induced fluorescence offers non-destructive and direct imaging of the THz field, providing real-time, single shot images. Second, we convert narrowband terahertz photons to infrared photons with 6% quantum efficiency allowing us to use nano-Watts of THz power to control micro-Watts of laser power on microsecond timescales. Exploiting hysteresis and a room-temperature phase transition in the response of the medium, we demonstrate a latching optical memory for sub pico-Joule THz pulses.

  2. Effects of external fields, dimension and polarization on the resonance fluorescence of quantum dots

    Science.gov (United States)

    Vaseghi, B.; Razavi, S. M.

    2017-02-01

    In this paper simultaneous effects of external electric and magnetic fields, dimension and polarization on the resonance fluorescence spectrum and photon statistics of a spherical quantum dot with parabolic confinement are investigated. With special attention to the optical scattering processes resonance fluorescence spectrum and second-order correlation function are calculated and plotted for different external parameters. Our results show the occurrence of resonance fluorescence similar to atomic systems and considerable effects of external fields, quantum confinement and light polarization on the resonance fluorescence spectrum and second-order correlation function in the quantum dot systems. The existence of Mollow triplets and photon antibunching are strongly depend on these external agents.

  3. Oxygen Atom Recombination in Carbon Dioxide Atmospheres

    Science.gov (United States)

    Jamieson, Corey; Garcia, R. M.; Pejakovic, D. A.; Kalogerakis, K. S.

    2009-09-01

    Understanding processes involving atomic oxygen is crucial for the study and modeling of composition, energy transfer, airglow, and transport dynamics in planetary atmospheres. Significant gaps and uncertainties exist in our understanding of the above processes, and often the relevant input from laboratory measurements is missing or outdated. We are conducting experiments to measure the rate coefficients for O + O + CO2 and O + O2 + CO2 recombination and investigate the O2 excited states produced following O-atom recombination. These laboratory measurements are key input for a quantitative understanding and reliable modeling of the atmospheres of the CO2 planets and their airglow. An ArF excimer laser with 193-nm pulsed output radiation is employed to partially photodissociate carbon dioxide. In an ambient-pressure (760 Torr) background of CO2, the O atoms produced recombine in a time scale of a few milliseconds. Detection of laser-induced fluorescence at 845 nm following two-photon excitation near 226 nm monitors the decay of the oxygen atom population. From the temporal evolution of the signal we can extract the rate coefficients for recombination of O + O and O + O2 in the presence of CO2. We also use fluorescence and resonance-enhanced multi-photon ionization techniques to detect the products of the O-atom recombination and subsequent relaxation in CO2. This work is supported by the US National Science Foundation's (NSF) Planetary Astronomy Program. Rosanne Garcia's participation was funded by the NSF Research Experiences for Undergraduates (REU) Program.

  4. Long range intermolecular forces in triatomic systems: connecting the atom-diatom and atom-atom-atom representations

    OpenAIRE

    2005-01-01

    The long-range forces that act between three atoms are analysed in both atom-diatom and atom-atom-atom representations. Expressions for atom-diatom dispersion coefficients are obtained in terms of 3-body nonadditive coefficients. The anisotropy of atom-diatom C_6 dispersion coefficients arises primarily from nonadditive triple-dipole and quadruple-dipole forces, while pairwise-additive forces and nonadditive triple-dipole and dipole-dipole-quadrupole forces contribute significantly to atom-di...

  5. FLEX: fluorescence explorer

    NARCIS (Netherlands)

    Stoll, M.Ph.; Court, A.J.; Smorenburg, C.; Visser, H.; Crocco, L.; Heilimo, J.; Honig, A.

    1999-01-01

    FLEX is a scientifically driven space mission to provide demonstration/validation of the instrumentation and technique for measuring the natural fluorescence of vegetation in the Fraunhofer lines. The payload consists of high spectral resolution (0.1-0.3 nm) CCD imaging grating spectrometer with two

  6. Fluorescence Experiments with Quinine

    Science.gov (United States)

    O'Reilly, James E.

    1975-01-01

    Describes a series of experiments which illustrate the analytical capabilities of fluorescence, and outlines two straightforward analyses involving real analyses. These experiments are suitable for an undergraduate instrumental analysis course and require approximately six to seven hours of laboratory time. (MLH)

  7. Prospects of Optical Single Atom Detection for Nuclear Astrophysics

    Science.gov (United States)

    Singh, Jaideep

    2015-10-01

    We will discuss the prospects of optically detecting single atoms captured in a cryogenic thin film of a noble gas such as neon. This proposed detection scheme, when coupled with a recoil separator, could be used to measure rare nuclear reactions relevant for nuclear astrophysics. In particular, we will focus on the 22Ne(α, n)25Mg reaction, which is an important source of neutrons for the s-process. Noble gas solids are an attractive medium because they are optically transparent and provide efficient, pure, stable, & chemically inert confinement for a wide variety of atomic and molecular species. Atoms embedded inside of noble gas solids have a fluorescence spectrum that is often significantly shifted from its absorption spectrum. This makes possible the detection of individual fluorescence photons against a background of intense excitation light, which can be suppressed using the appropriate optical filters. We will report on our efforts to optically detect single Yb atoms in solid Ne. Yb is an ideal candidate for initial studies because it emits a strong green fluorescence when excited by blue light and it has an atomic structure that very closely resembles that of Mg. This work is supported by funds from Michigan State University.

  8. Determination of arsenic in antimony ingot and antimony trioxide by hydride generation-atomic fluorescence spectrometry%氢化物发生-原子荧光光谱法测定锑锭及三氧化二锑中的砷

    Institute of Scientific and Technical Information of China (English)

    钱光敏; 赵国杏

    2012-01-01

    The antimony slab and antimonous oxide samples were dissolved by sulfuric acid and hydrochloric acid, respectively. The Sb3+ in solution was precipitated with sodium hydroxide to separate trace arsenic from matrix antimony. The thiourea-ascorbic acid was added to reduce As5+ to As3+. Then, the arsenic in antimony slab and antimonous oxide was determined by atomic fluorescence spec-trometry. The hydride generation conditions were investigated: the concentration of reducing agent potassium borohydride was 25 g/L, the determination medium was 20% (V/V) hydrochloric acid, and the dosage of thiourea - ascorbic acid solution was 5 mL. The interference test of coexisting elements showed that, the interference of residual antimony in solution after precipitation could be fully eliminated by adding 1 mL of tartaric acid solution. Other impurity elements in sample did not interfere with the determination of arsenic after adding thiourea-ascorbic acid solution. The detection limit of method was 0. 156 ng/mL. The antimony slab and antimonous oxide samples were analyzed by the proposed method, and the relative standard deviation (RSD) was 0. 95%-1.2%. The determination results were consistent with those obtained by national standard methods.%采用硫酸溶解锑锭样品,盐酸溶解三氧化二锑样品,用氢氧化钠溶液使Sb3+沉淀从而使基体锑与微量砷分离,通过加入硫脲-抗坏血酸将As5+还原成As3+,然后在原子荧光仪上测定锑锭及三氧化二锑中的砷.对氢化物发生条件进行考察,确定还原剂硼氢化钾的浓度为25 g/L、测定介质为20%(V/V)盐酸、硫脲-抗坏血酸溶液用量为5 mL.共存元素干扰试验表明,沉淀后溶液中残留少量锑的干扰在加入1 mL酒石酸溶液后可以完全消除,而样品中其他杂质元素在加入硫脲-抗坏血酸溶液后不干扰砷的测定.方法的检出限为0.156 ng/mL.对锑锭及三氧化二锑样品进行分析,相对标准偏差为0.95%~1.2%,测定

  9. Determination of Water Soluble As ( Ⅲ ) and As ( Ⅴ ) in Soil by Hydride Generation-Atomic Fluorescence Spectrometry%氢化物发生-原子荧光光谱法测定土壤中水溶态砷(Ⅲ)和砷(Ⅴ)

    Institute of Scientific and Technical Information of China (English)

    于兆水; 张勤; 刘玲

    2012-01-01

    以氢气发生器为氩-氢火焰提供纯净、稳定的氢气,原子荧光光谱法测定土壤中水溶态和可交换态Sb(Ⅲ)和Sb(Ⅴ)已有应用,本研究进一步将此方法用于测定土壤样品中的As(Ⅲ)和As(Ⅴ).在0.3mol/L NaH2PO4 - Na2HPO4缓冲液中,采用氢化物发生-原子荧光光谱法测定土壤中水溶态As(Ⅲ)和总砷的含量,通过差减法计算As(Ⅴ)的含量.实验考察了0.02~0.4 mol/L NaH2PO4 - Na2 HPO4对As(Ⅲ)和As(Ⅴ)测定的影响,结果表明0.3 mol/L NaH2PO4 - Na2HPO4可以有效掩蔽As(Ⅴ).As(Ⅲ)的检出限为2.92 ng/g,总砷的检出限为2.35 ng/g;As(Ⅲ)和As(Ⅴ)的加标回收率分别为96% ~ 104%和101% ~103%.本方法不再依靠化学反应产生氢气来点燃并维持氩氢火焰,可在发生氢化反应的任何介质中测定砷,且不需要考虑酸度问题.方法操作简便,准确度高,能满足大批量样品分析要求.%Based on the determination method of Sb ( HI) and Sb ( V ) in soil, a method for the determination of water soluble As ( M ) and total arsenic in soil has been established by using Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS) in the media of 0. 3 mol/L NaH2PO4-Na2HPO4. An amount of As( V ) was obtained by subtracting As( HI ) from total arsenic. The hydrogen was provided from a hydrogen generator instead of chemical reaction to ignite a H2-Ar flame. Therefore, arsenic in any media was measurable since the arsenic was reduced into AsH3. Effects on the determination of As ( M ) and As ( V ) were investigated for concentrations of NaH2PO4-Na2HPO4 from 0. 02 mol/L to 0. 4 mol/L. The results show As( V ) can be screened by 0. 3 mol/L NaH2PO4-Na2HPO4. The detection limits were 2. 92 ng/g for As( HJ ) and 2. 35 ng/g for total As. The recoveries of As( HI) and As( V ) are 96% - 104% and 101% - 103% , respectively. The method was simple and highly accurate, meeting the requirements for multiple sample analysis.

  10. THE DETERMINATION OF ANTIMONY (Ⅲ) AND ANTOMONY (Ⅴ) IN GEOLOGICAL SAMPLES BY HYDRIDE GENERATION-ATOMIC FLUORESCENCE SPECTROMETRY%氢化物发生—原子荧光光谱法测定地质样品中的锑(Ⅲ)和锑(Ⅴ)

    Institute of Scientific and Technical Information of China (English)

    郝志红; 杨帆; 刑夏; 汤志勇; 张勤

    2012-01-01

    A method for the determination of antimony ( Ⅲ ) and antimony ( V ) in geological samples (stream sediments) by hydride generation-atomic fluorescence spectrometry was developed in the paper. 4. 8 mol/L HC1 could be used as the extraclant with ultrasonic-assisted extraction. In the medium of 0. 24 mol/L hydrochloric acid, antimony ( Ⅲ) could be alternatively determined with 6 g/mL sodium citrate as the masking agent for Sb (V). Then antimony ( V ) could be figured out by the subtraction method. The detection limit of the method was 0. 075 × 10 -6 for Sb ( 1) and 0. 097 × 10 -6 for Sb ( V ) , and the relative standard deviation was 1. 1 % and 0. 64% ( n = 11) for 40 ng/mL Sb ( Ⅲ ) and 40 ng/mL Sb( V ) standard solution. The proposed method was applied to the determination of antimony ( Ⅲ) and antimony ( V ) in geological samples, and a comparison between the extraction results and the aqua regia dissolution results shows that the extraction rate of antimony was higher than 80% , the recoveries were in the ranges of 83% - 107% and 98% -114% for Sb ( Ⅲ) and Sb (V) respectively.%提出了一种氢化物发生—原子荧光光谱法测定地质样品(水系沉积物)中Sb(Ⅲ)和Sb(Ⅴ)的方法.选取4.8 mol/L HC1为提取剂,采用超声波辅助提取,以6 g/mL柠檬酸钠作为Sb(Ⅴ)的掩蔽剂,在0.24 mol/L的HC1介质中选择性测定Sb(Ⅲ),用差减法求得Sb(Ⅴ).Sb(Ⅲ)的方法检出限为0.075×10-6,Sb(Ⅴ)的方法检出限为0.097×10-6.对40 ng/mL的Sb(Ⅲ)和Sb(Ⅴ)分别连续测定11次,得到相对标准偏差分别为1.1%和0.64%.应用该方法对地质样品中的Sb(Ⅲ)和Sb(Ⅴ)进行分析测定,并与王水溶解值相比较,该方法测定的总Sb提取率在80%以上,Sb(Ⅲ)和Sb(Ⅴ)的加标回收率分别为83% ~ 107%和98% ~ 114%.

  11. 水产品中甲基汞测定的液相色谱-原子荧光光谱联用方法的改进%Improvement of the method for methylmercury determination in aquatic products using liquid chromatography online coupled with atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    尚晓虹; 赵云峰; 张磊; 李筱薇; 吴永宁

    2011-01-01

    The improvement method was developed for methylmercury determination using liquid chromatography online coupled with cold vapor atomic fluorescence spectrometry ( LC-CVAFS ). Cysteine was used as complexing agent in mobile phase instead of mercaptoethanol.Under the optimized conditions , baseline separation of mercury species could be achieved within 8 min on a C18 column with a mobile phase of 5% ( V/V ) acetonitrile-1 g/L L-cysteine-50 mmol/L ammonium acetate aqueous solution. The linear range of calibration curve of methyl-mercury was 1 - 50 μg/L and the limit of detection ( S/N = 3 ) for methylmercury was 0.3 μg/L.Ultrasonication assisted hydrochloric acid extraction was used to extract methylmercury from seafood samples. The sample extract was cleaned up by a C18 solid phase extraction ( SPE )cartridge. For validation of the method, certified reference materials and spiked seafood samples were analyzed. The determined methylmercury contents of certified reference materials NIST1566b、BCR464 and GBW10029 agreed well with the certified values. The determined methylmercury values for Food Analysis Performance Assessment Scheme ( FAPAS ) sample 07115 were satisfied. The recoveries of methylmercury in seafood samples at three spiked levels ( 10,50 and 500 μg/kg ) ranged from 89% to 112% , including cooked seafood food. The precision of the method based on relative standard deviation ( RSD ) was not more than 7%. The present method of LC-CV-AFS is accurate, sensitive, simple, and can meet the demand of methylmer-cury determination in seafood.%对本实验室前期建立的食品中甲基汞的液相色谱-原子荧光光谱联用测定方法进行了改进.采用无毒的半胱氨酸代替有毒试剂巯基乙醇作为流动相中的配位剂,流动相组成为5%(v/v)乙腈-1 g/L半胱氨酸-50 mmol/L乙酸铵水溶液,使汞化合物分离时间缩短至8 min.在优化条件下,甲基汞标准曲线的线性范围为1~50 μg/L,检出限(S/V=3)为0/3

  12. Determination of Mercuryalkylide in Water Using High Performance Liquid Chromatography with Hydride Generation Atomic Fluorescence Detection%高效液相色谱-氢化物发生-原子荧光光谱联用技术测定水中烷基汞

    Institute of Scientific and Technical Information of China (English)

    陈邵鹏; 顾海东; 秦宏兵

    2012-01-01

    A method for the determination of Mercury species in both surface water and waste water was established by high performance liquid chromatography ( HPLC ) -hydride generation ( HG) -atomic fluorescence spectrophotometry ( AFS). Sample was extracted by dichloromethane, subsequently back-extracted by mixed extractant containing cysteine and ammonium acetate before HPLC-HG-AFS detection. Under the optimized conditions, both methyl mercury and ethyl mercury responded linearly in the concentration of 1-50μg/L. The recoveries for both standard samples and actual samples were 80%-110%. The relative standard deviations for the determination of methyl and ethylmercury with the concentration of 1μg/L were 5. 2% and 3. 9% , respectively. The detection limits for them were 0.4 ng/L and 0.7 ng/L, respectively with the American EPA methord. The proposed method is of good accuracy, high repeatability, precision, less interferences from impurities and low cost, which is benefit for expanding and applying in the common laboratory.%建立了高效液相色谱(HPLC)-氢化物发生(HG)-原子荧光光谱(AFS)联用技术分析地表水及废水中甲基汞和乙基汞的方法.样品经二氯甲烷萃取,再以半胱氨酸+乙酸铵溶液反萃取富集,并进入高效液相色谱分离,经形态分析预处理装置后,借助原子荧光光谱法检测.在优化分离条件下,甲基汞和乙基汞在1 ~ 50 μg/L范围内呈现良好的线性关系,对于标准水样、地表水和废水实际水样,加标平均回收率均为80% ~ 110%.平行进样7次1μg/L的汞混合标准溶液,甲基汞和乙基汞的色谱峰面积的相对标准偏差分别为5.2%和3.9%,检出限则分别为0.4 ng/L和0.7 ng/L.该检测方法前处理简单、回收率稳定、灵敏度和准确度高、检出限低、杂质干扰少、监测费用低,便于在普通实验室推广和应用.

  13. Determination of Lead in Tea Garden Soil by Hydride Generation Atomic Fluorescence Spectrometry with Microwave Digestion%微波消解-氢化物发生原子荧光光谱法测定茶园土壤中的铅

    Institute of Scientific and Technical Information of China (English)

    凤海元; 时晓露; 黄勤

    2013-01-01

    样品用王水微波消解浸提,氢化物发生-原子荧光光谱法测定茶园土壤中痕量铅的含量.对样品浸取方法、实验条件、增感剂和共存元素进行了条件实验.结果表明,王水微波消解浸取,铅浸出量最大,减少了试剂用量和环境污染;铁氰化钾-盐酸羟胺体系有显著的增感作用,铁氰化钾在配制溶液时用米糠除去试剂中可能存在的铅,降低了空白;钴、锌、砷、镉等共存离子不干扰铅的测定,通过加入邻菲啰啉-硫氰酸钠消除铁和铜的干扰,提高了铅的回收率.方法检出限为0.65 μg/L,精密度(RSD,n=10)为1.89%,回收率在86.8% ~ 110.4%之间.用土壤标准物质验证,测定值与标准值相符,方法快速准确,适合于大批量样品的分析检测.%The microwave digestion system with aqua regia was developed for the determination of trace lead in tea garden soil using Hydride Generation-Atomic Fluorescence Spectrometry ( HG-AFS). The leaching methods, experimental conditions, booster and coexisting element were optimized. The largest amount of lead was leached out by microwave digestion with aqua regia, which has the advantages of less usage of reagent and less environmental pollution. An appropriate amount of potassium ferricyanide and hydroxylamine hydrochloride improved the hydride generation efficiency of Pb. The lead blank was reduced significantly when Potassium ferricyanide solution was treated with rice husk to remove Pb in the reagent. It was found that Co, Zn, As, and Cd did not interfere with the determination of lead. The addition of 1,10-phenanthroline monohydrate and sodium hydrosulfide could effectively eliminate the interferences from Fe and Cu, which improved the recovery rate of lead. The limit of detection was 0. 65 μg/L and the precision was 1. 89% (n = 10) with recoveries of 86. 8% - 110. 4% for Pb. The reliability of the method has been tested by determination of Pb in the Soils Standard Reference

  14. NANODIAMONDS FOR FLUORESCENT CELL AND SENSOR NANOTECHNOLOGIES

    Directory of Open Access Journals (Sweden)

    V. I. Nazarenko

    2013-10-01

    Full Text Available This review addresses the analysis of properties and applications of fluorescent nanodiamonds. They are carbon nanostructures with atomic arrangement of a diamond and carry all its properties, including record — high density, rigidity and refraction index. They are of almost spherical shape, and their small size (~4–10 nm creates substantial surface area that can be used for absorption of different compounds including drugs. Their surface is formed by different chemical groups (hydroxyls, carboxyls, etc. exhibits also chemical reactivity that allows different types of modifications. This opens innumerable possibilities for constructing different functional nanomaterials. The technologies have been developed for making these nanodiamonds fluorescent. Particularly, these properties are achieved by radioactive treatment with the formation of N–V impurities. These particles absorb and emit light in convenient for observation visible range of spectrum. They do not photobleach, which is very attractive for fluorescent microscopy of the cell. And, finally, these nanoparticles do not display toxicity on the cellular or whole — body level, and because of their biocompatibility they can be used in vivo as contrast agents and drug carriers. It is expected that future biotechnological applications of these nanoparticles will be connected with the creation of nanocomposites that combine multiple useful functions.

  15. Determination of ruthenium in pharmaceutical compounds by graphite furnace atomic absorption spectroscopy.

    Science.gov (United States)

    Jia, Xiujuan; Wang, Tiebang; Bu, Xiaodong; Tu, Qiang; Spencer, Sandra

    2006-04-11

    A graphite furnace atomic absorption (GFAA) spectrometric method for the determination of ruthenium (Rh) in solid and liquid pharmaceutical compounds has been developed. Samples are dissolved or diluted in dimethyl sulfoxide (DMSO) without any other treatment before they were analyzed by GFAA with a carefully designed heating program to avoid pre-atomization signal loss and to achieve suitable sensitivity. Various inorganic and organic solvents were tested and compared and DMSO was found to be the most suitable. In addition, ruthenium was found to be stable in DMSO for at least 5 days. Spike recoveries ranged from 81 to 100% and the limit of quantitation (LOQ) was determined to be 0.5 microg g(-1) for solid samples or 0.005 microg ml(-1) for liquid samples based a 100-fold dilution. The same set of samples was also analyzed by ICP-MS with a different sample preparation method, and excellent agreement was achieved.

  16. Atomic homodyne detection of weak atomic transitions.

    Science.gov (United States)

    Gunawardena, Mevan; Elliott, D S

    2007-01-26

    We have developed a two-color, two-pathway coherent control technique to detect and measure weak optical transitions in atoms by coherently beating the transition amplitude for the weak transition with that of a much stronger transition. We demonstrate the technique in atomic cesium, exciting the 6s(2)S(1/2) --> 8s(2)S(1/2) transition via a strong two-photon transition and a weak controllable Stark-induced transition. We discuss the enhancement in the signal-to-noise ratio for this measurement technique over that of direct detection of the weak transition rate, and project future refinements that may further improve its sensitivity and application to the measurement of other weak atomic interactions.

  17. The Software Atom

    CERN Document Server

    Javanainen, Juha

    2016-01-01

    By putting together an abstract view on quantum mechanics and a quantum-optics picture of the interactions of an atom with light, we develop a corresponding set of C++ classes that set up the numerical analysis of an atom with an arbitrary set of angular-momentum degenerate energy levels, arbitrary light fields, and an applied magnetic field. As an example, we develop and implement perturbation theory to compute the polarizability of an atom in an experimentally relevant situation.

  18. The Software Atom

    Science.gov (United States)

    Javanainen, Juha

    2017-03-01

    By putting together an abstract view on quantum mechanics and a quantum-optics picture of the interactions of an atom with light, we develop a corresponding set of C++ classes that set up the numerical analysis of an atom with an arbitrary set of angular-momentum degenerate energy levels, arbitrary light fields, and an applied magnetic field. As an example, we develop and implement perturbation theory to compute the polarizability of an atom in an experimentally relevant situation.

  19. Advances in atomic spectroscopy

    CERN Document Server

    Sneddon, J

    1997-01-01

    This series describes selected advances in the area of atomic spectroscopy. It is primarily intended for the reader who has a background in atmoic spectroscopy; suitable to the novice and expert. Although a widely used and accepted method for metal and non-metal analysis in a variety of complex samples, Advances in Atomic Spectroscopy covers a wide range of materials. Each Chapter will completely cover an area of atomic spectroscopy where rapid development has occurred.

  20. Advances in atomic spectroscopy

    CERN Document Server

    Sneddon, J

    1995-01-01

    This series describes selected advances in the area of atomic spectroscopy. It is promarily intended for the reader who has a background in atmoic spectroscopy; suitable to the novice and expert. Although a widely used and accepted method for metal and non-metal analysis in a variety of complex samples, Advances in Atomic Spectroscopy covers a wide range of materials. Each Chapter will completely cover an area of atomic spectroscopy where rapid development has occurred.

  1. Atomicity in Electronic Commerce,

    Science.gov (United States)

    1996-01-01

    tremendous demand for the ability to electronically buy and sell goods over networks. Electronic commerce has inspired a large variety of work... commerce . It then briefly surveys some major types of electronic commerce pointing out flaws in atomicity. We pay special attention to the atomicity...problems of proposals for digital cash. The paper presents two examples of highly atomic electronic commerce systems: NetBill and Cryptographic Postage Indicia.

  2. Dephasing in an atom

    OpenAIRE

    2011-01-01

    When an atom in vacuum is near a surface of a dielectric the energy of a fluctuating electromagnetic field depends on a distance between them resulting, as known, in the force called van der Waals one. Besides this fluctuation phenomenon there is one associated with formation of a mean electric field which is equivalent to an order parameter. In this case atomic electrons are localized within atomic distances close to the atom and the total ground state energy is larger, compared to the bare ...

  3. Synthesis and Fluorescence Spectra of Triazolylcoumarin Fluorescent Dyes

    Institute of Scientific and Technical Information of China (English)

    PENG Xian-fu; LI Hong-qi

    2009-01-01

    Much attention is devoted to fluorescent dyes especially those with potential in versatile applications. Reactions under "click" conditions between nonfluorescent 3 - azidocoumarins and terminal alkynes produced 3 -(1, 2, 3- triazol- 1 - yl)cournarins, a novel type of fluorescent dyes with intense fluorescence. The structures of the new coumarins were characterized by 1H NMR, MS, and IR spectra. Fluorescence spectra measurement demonstrated excellent fluorescence performance of the triazolylcoumarins and this click reaction is a promising candidate for bioconjugation and bioimaging applications since both azide and alkynes are quite inert to biological systems.

  4. Fluorescence nanoscopy. Methods and applications

    OpenAIRE

    Requejo-Isidro, Jose

    2013-01-01

    Fluorescence nanoscopy refers to the experimental techniques and analytical methods used for fluorescence imaging at a resolution higher than conventional, diffraction-limited, microscopy. This review explains the concepts behind fluorescence nanoscopy and focuses on the latest and promising developments in acquisition techniques, labelling strategies to obtain highly detailed super-resolved images and in the quantitative methods to extract meaningful information from them.

  5. Rydberg atom detection of the temporal coherence of cosmic microwave background radiation

    CERN Document Server

    Tscherbul, Timur V

    2013-01-01

    Rydberg atoms immersed in cold blackbody radiation are shown to display long-lived quantum coherence effects on timescales of tens of picoseconds. By solving non-Markovian equations of motion with no free parameters we obtain the time evolution of the density matrix, and demonstrate that the blackbody-induced temporal coherences manifest as quantum beats in time-resolved fluorescence intensities of the Rydberg atoms. A measurable fluorescence signal can be obtained with a cold trapped ensemble of 1e8 Rydberg atoms subject to 2.7 K cosmic microwave background radiation (CMB), allowing for novel insights into previously unexamined quantum coherence properties of CMB.

  6. Single molecule DNA detection with an atomic vapor notch filter

    Energy Technology Data Exchange (ETDEWEB)

    Uhland, Denis; Rendler, Torsten; Widmann, Matthias; Lee, Sang-Yun [University of Stuttgart and Stuttgart Research Center of Photonic Engineering (SCoPE) and IQST, 3rd Physics Institute, Stuttgart (Germany); Wrachtrup, Joerg; Gerhardt, Ilja [University of Stuttgart and Stuttgart Research Center of Photonic Engineering (SCoPE) and IQST, 3rd Physics Institute, Stuttgart (Germany); Max Planck Institute for Solid State Research, Stuttgart (Germany)

    2015-12-01

    The detection of single molecules has facilitated many advances in life- and material-science. Commonly the fluorescence of dye molecules is detected, which are attached to a non-fluorescent structure under study. For fluorescence microscopy one desires to maximize the detection efficiency together with an efficient suppression of undesired laser leakage. Here we present the use of the narrow-band filtering properties of hot atomic sodium vapor to selectively filter the excitation light from the red-shifted fluorescence of dye labeled single-stranded DNA molecules. A statistical analysis proves an enhancement in detection efficiency of more than 15% in a confocal and in a wide-field configuration. (orig.)

  7. Evanescent Wave Atomic Mirror

    Science.gov (United States)

    Ghezali, S.; Taleb, A.

    2008-09-01

    A research project at the "Laboratoire d'électronique quantique" consists in a theoretical study of the reflection and diffraction phenomena via an atomic mirror. This poster presents the principle of an atomic mirror. Many groups in the world have constructed this type of atom optics experiments such as in Paris-Orsay-Villetaneuse (France), Stanford-Gaithersburg (USA), Munich-Heidelberg (Germany), etc. A laser beam goes into a prism with an incidence bigger than the critical incidence. It undergoes a total reflection on the plane face of the prism and then exits. The transmitted resulting wave out of the prism is evanescent and repulsive as the frequency detuning of the laser beam compared to the atomic transition δ = ωL-ω0 is positive. The cold atomic sample interacts with this evanescent wave and undergoes one or more elastic bounces by passing into backward points in its trajectory because the atoms' kinetic energy (of the order of the μeV) is less than the maximum of the dipolar potential barrier ℏΩ2/Δ where Ω is the Rabi frequency [1]. In fact, the atoms are cooled and captured in a magneto-optical trap placed at a distance of the order of the cm above the prism surface. The dipolar potential with which interact the slow atoms is obtained for a two level atom in a case of a dipolar electric transition (D2 Rubidium transition at a wavelength of 780nm delivered by a Titane-Saphir laser between a fundamental state Jf = l/2 and an excited state Je = 3/2). This potential is corrected by an attractive Van der Waals term which varies as 1/z3 in the Lennard-Jones approximation (typical atomic distance of the order of λ0/2π where λ0 is the laser wavelength) and in 1/z4 if the distance between the atom and its image in the dielectric is big in front of λ0/2π. This last case is obtained in a quantum electrodynamic calculation by taking into account an orthornormal base [2]. We'll examine the role of spontaneous emission for which the rate is inversely

  8. Atomic transition probabilities of Gd i

    Science.gov (United States)

    Lawler, J. E.; Bilty, K. A.; Den Hartog, E. A.

    2011-05-01

    Fourier transform spectra are used to determine emission branching fractions for 1290 lines of the first spectrum of gadolinium (Gd i). These branching fractions are converted to absolute atomic transition probabilities using previously reported radiative lifetimes from time-resolved laser-induced-fluorescence measurements (Den Hartog et al 2011 J. Phys. B: At. Mol. Opt. Phys. 44 055001). The wavelength range of the data set is from 300 to 1850 nm. A least squares technique for separating blends of the first and second spectra lines is also described and demonstrated in this work.

  9. Atomic transition probabilities of Er i

    Science.gov (United States)

    Lawler, J. E.; Wyart, J.-F.; Den Hartog, E. A.

    2010-12-01

    Atomic transition probabilities for 562 lines of the first spectrum of erbium (Er i) are reported. These data are from new branching fraction measurements on Fourier transform spectra normalized with previously reported radiative lifetimes from time-resolved laser-induced fluorescence measurements (Den Hartog et al 2010 J. Phys. B: At. Mol. Opt. Phys. 43 155004). The wavelength range of the data set is from 298 to 1981 nm. In this work we explore the utility of parametric fits based on the Cowan code in assessing branching fraction errors due to lines connecting to unobserved lower levels.

  10. Atomic transition probabilities of Nd I

    Science.gov (United States)

    Stockett, M. H.; Wood, M. P.; Den Hartog, E. A.; Lawler, J. E.

    2011-12-01

    Fourier transform spectra are used to determine emission branching fractions for 236 lines of the first spectrum of neodymium (Nd i). These branching fractions are converted to absolute atomic transition probabilities using radiative lifetimes from time-resolved laser-induced fluorescence measurements (Den Hartog et al 2011 J. Phys. B: At. Mol. Opt. Phys. 44 225001). The wavelength range of the data set is from 390 to 950 nm. These transition probabilities from emission and laser measurements are compared to relative absorption measurements in order to assess the importance of unobserved infrared branches from selected upper levels.

  11. Sensitive spectroscopy of an ytterbium atomic beam

    CERN Document Server

    Guttridge, A; Kemp, S L; Boddy, D; Freytag, R; Tarbutt, M R; Hinds, E A; Cornish, S L

    2015-01-01

    Experimental studies of ultracold ytterbium atoms generally involve the frequency stabilisation (locking) of lasers to two transitions at 399 and 556 nm in order to implement laser cooling. Here we present a simple and robust apparatus for generation of suitable, narrow fluorescence signals with a high signal to noise ratio at both wavelengths. The design utilises easily acquired vacuum parts, optics and electronics and requires very little laser power. We demonstrate the stability and precision of the frequency stabilisation at 556 nm by presenting sensitive measurements of the gravitational sag of an ytterbium MOT as a function of laser power.

  12. Functionalization of hydroxyl terminated polybutadiene with biologically active fluorescent molecule

    Indian Academy of Sciences (India)

    R Murali Sankar; Subhadeep Saha; K Seeni Meera; Tushar Jana

    2009-10-01

    A biologically active molecule, 2-chloro-4,6-bis(dimethylamino)-1,3,5-triazine (CBDT), has been covalently attached at the terminal carbon atoms of the hydroxyl terminated polybutadiene (HTPB) backbone. The modification of HTPB backbone by CBDT molecule does not affect the unique physico-chemical properties such as fluidity, hydroxyl value and microstructure of the parent HTPB. The formation of hydrogen bonding between the terminal hydroxyl groups and the nitrogen atoms of triazine moiety is the driving force for the terminal attachment chemistry. The functionalized HTPB (HTPB–CBDT) shows a strong fluorescence emission at 385 nm.

  13. Fluorescent Thiol-Derivatized Gold Clusters Embedded in Polymers

    Directory of Open Access Journals (Sweden)

    G. Carotenuto

    2013-01-01

    Full Text Available Owing to aurophilic interactions, linear and/or planar Au(I-thiolate molecules spontaneously aggregate, leading to molecular gold clusters passivated by a thiolate monolayer coating. Differently from the thiolate precursors, such cluster compounds show very intensive visible fluorescence characteristics that can be tuned by alloying the gold clusters with silver atoms or by conjugating the electronic structure of the metallic core with unsaturated electronic structures in the organic ligand through the sulphur atom. Here, the photoluminescence features of some examples of these systems are shortly described.

  14. Mass spectrometric identification of an azobenzene derivative produced by smectite-catalyzed conversion of 3-amino-4-hydroxyphenylarsonic acid

    Science.gov (United States)

    Wershaw, R. L.; Rutherford, D.W.; Rostad, C.E.; Garbarino, J.R.; Ferrer, I.; Kennedy, K.R.; Momplaisir, G.-M.; Grange, A.

    2003-01-01

    The compound 3-amino-4-hydroxyphenylarsonic acid (3-amino-HPAA) reacts with smectite to form a soluble azobenzene arsonic acid compound. This reaction is of particular interest because it provides a possible mechanism for the formation of a new type of arsenic compound in natural water systems. 3-Amino-HPAA is a degradation product excreted by chickens that are fed rations amended with roxarsone. Roxarsone is used to control coccidial intestinal parasites in most of the broiler chickens grown in the United States. The structure of the azobenzene arsonic acid compound was first inferred from negative-ion and positive-ion low-resolution mass-spectrometric analyses of the supernatant of the smectite suspension. Elemental composition of the parent ion determined by high-resolution positive-ion mass spectrometric measurements was consistent with the proposed structure of the azobenzene arsonic acid compound. Published by Elsevier Science B.V.

  15. 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...

  16. Control of light trapping in a large atomic system by a static magnetic field

    CERN Document Server

    Skipetrov, S E; Havey, M D

    2016-01-01

    We propose to control light trapping in a large ensemble of cold atoms by an external, static magnetic field. For an appropriate choice of frequency and polarization of the exciting pulse, the field is expected to speed up the fluorescence of a dilute atomic system but can significantly slow it down in a dense ensemble. The slowing down of fluorescence is due to the excitation of spatially localized collective atomic states that appear only under a strong magnetic field and have exponentially long lifetimes. The control of fluorescence by the magnetic field may be of interest for use in future quantum-information processing devices. It also paves a way towards the experimental observation of the disorder-induced localization of light in cold atomic systems.

  17. Spectrometric studies on the interaction of fluoroquinolones and bovine serum albumin

    Science.gov (United States)

    Ni, Yongnian; Su, Shaojing; Kokot, Serge

    2010-02-01

    The interaction between fluoroquinolones (FQs), ofloxacin and enrofloxacin, and bovine serum albumin (BSA) was investigated by fluorescence and UV-vis spectroscopy. It was demonstrated that the fluorescence quenching of BSA by FQ is a result of the formation of the FQ-BSA complex stabilized, in the main, by hydrogen bonds and van der Waals forces. The Stern-Volmer quenching constant, KSV, and the corresponding thermodynamic parameters, Δ H, Δ S and Δ G, were estimated. The distance, r, between the donor, BSA, and the acceptor, FQ, was estimated from fluorescence resonance energy transfer (FRET). The effect of FQ on the conformation of BSA was analyzed with the aid of UV-vis absorbance spectra and synchronous fluorescence spectroscopy. Spectral analysis showed that the two FQs affected the conformation of the BSA but in a different manner. Thus, with ofloxacin, the polarity around the tryptophan residues decreased and the hydrophobicity increased, while for enrofloxacin, the opposite effect was observed.

  18. Chromatographic isolation and mass spectrometric identification of a base-induced mebendazole fluorophor.

    Science.gov (United States)

    Baeyens, W; Abdel Fattah, F; De Moerloose, P

    1986-10-01

    Sodium hydroxide treatment of the benzoylbenzimidazole anthelmintics mebendazole and flubendazole produces yellow solutions that possess practically no fluorescence characteristics under various conditions. However, when spotting the alkaline solutions on filter paper and examining the spots under U.V., strong bluish-white fluorescence is obtained. When pouring liquid nitrogen over the spots, a very intense bluish-white fluorescence followed by a long-lasting greenish phosphorescence is observed. These luminescence phenomena allow visualization of 1 ng of mebendazole and of 5 ng of flubendazole per spot. A preparative separation by means of column liquid chromatography was worked out for the isolation of the fluorophor in case of mebendazole. Combined spectroscopic methods indicated the formation of a primary amine function in position 2 of the imidazole nucleus by hydrolytic cleavage of the -NH-CO-bond. A discussion on the mechanism of fluorescence is given.

  19. Greek Atomic Theory.

    Science.gov (United States)

    Roller, Duane H. D.

    1981-01-01

    Focusing on history of physics, which began about 600 B.C. with the Ionian Greeks and reaching full development within three centuries, suggests that the creation of the concept of the atom is understandable within the context of Greek physical theory; so is the rejection of the atomic theory by the Greek physicists. (Author/SK)

  20. Atoms, Molecules, and Compounds

    CERN Document Server

    Manning, Phillip

    2007-01-01

    Explores the atoms that govern chemical processes. This book shows how the interactions between simple substances such as salt and water are crucial to life on Earth and how those interactions are predestined by the atoms that make up the molecules.