WorldWideScience

Sample records for atomic fluorescence spectrometric

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

    International Nuclear Information System (INIS)

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

  2. Instrumental modification intended to save time, and volumes of sample and reagent solutions, in the atomic fluorescence spectrometric determination of mercury.

    Science.gov (United States)

    Pérez-Sirvent, Carmen; Martínez-Sánchez, María J; García-Lorenzo, Mariluz; López-García, Ignacio; Hernández-Córdoba, Manuel

    2007-05-01

    Use of small membrane pumps, instead of peristaltic pumps, to introduce sample and reagent solutions into the spectrometer has several advantages in atomic fluorescence spectrometric determination of mercury. This simple modification results in a substantial saving in the time required for the measurements and so 90% of reagent solution volumes and 95% of sample solution volumes are saved, with a consequent decrease in the volume of waste generated. The sampling frequency is almost tripled, with no deterioration in sensitivity, which is similar to that obtained by use of peristaltic pumps. The relative standard deviation for ten consecutive measurements of a 1 microg L-1 mercury solution was approximately 2%. PMID:17351707

  3. 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.

  4. 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

  5. Hydride generation atomic fluorescence spectrometric determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter using multivariate optimization

    Energy Technology Data Exchange (ETDEWEB)

    Moscoso-Perez, Carmen [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Moreda-Pineiro, Jorge [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain)]. E-mail: jmoreda@udc.es; Lopez-Mahia, Purificacion [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Muniategui-Lorenzo, Soledad [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Fernandez-Fernandez, Esther [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Prada-Rodriguez, Dario [Department of Analytical Chemistry, Faculty of Sciences, University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain)

    2004-11-22

    A highly sensitive and simple method, based on hydride generation and atomic fluorescence detection, has been developed for the determination of As, Bi, Sb, Se(IV) and Te(IV) in aqua regia extracts from atmospheric particulate matter samples. Atmospheric particulates matter was collected on glass fiber filters using a medium volume sampler (PM1 particulate matter). Two-level factorial designs have been used to optimise the hydride generation atomic fluorescence spectrometry (HG-AFS) procedure. The effects of several parameters affecting the hydride generation efficiency (hydrochloric acid, sodium tetrahydroborate and potassium iodide concentrations and flow rates) have been evaluated using a Plackett-Burman experimental design. In addition, parameters affecting the hydride measurement (delay, analysis and memory times) have been also investigated. The significant parameters obtained (sodium tetrahydroborate concentration, sodium tetrahydroborate flow rate and analysis time for As; hydrochloric acid concentration and sodium tetrahydroborate flow rate for Se(IV); and sodium tetrahydroborate concentration and sodium tetrahydroborate flow rate for Te(IV)) have been optimized by using 2{sup n} + star central composite design. Hydrochloric acid concentration and sodium tetrahydroborate flow rate were the significant parameters obtained for Sb and Bi determination, respectively. Using a univariate approach these parameters were optimized. The accuracy of methods have been verified by using several certified reference materials: SRM 1648 (urban particulate matter) and SRM 1649a (urban dust). Detection limits in the range of 6 x 10{sup -3} to 0.2 ng m{sup -3} have been achieved. The developed methods were applied to several atmospheric particulate matter samples corresponding to A Coruna city (NW Spain)

  6. System for Gamma an X rays fluorescence spectrometric

    International Nuclear Information System (INIS)

    A system for spectrometry of gamma or fluorescence X rays is presented. It sis composed by a Si(Li) semiconductors detector, a charge sensitive preamplifier, a high voltage power supply, a spectrometric amplifier and a monolithic 1024 channels multichannel analyzers or an IBM compatible 4096 channels add - on- card multichannel analyzer. The system can be configured as a 1024 or 4096 channels gamma or fluorescent X rays spectrometer

  7. 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.

  8. Use of Ni/NixB Nanoparticles as a Novel Adsorbent for the Preconcentration of Mercury Species prior to Cold Vapor-Atomic Fluorescence Spectrometric Determination.

    Science.gov (United States)

    Yayayürük, Onur; Henden, Emür

    2016-01-01

    A selective matrix separation/enrichment method, utilizing a simple batch procedure with nickel/nickel boride (Ni/NixB) nanoparticles was proposed for the determination of inorganic mercury(II), Hg(2+) and methyl mercury(I), CH3Hg(+) in waters prior to cold vapor-atomic fluorescence spectrometry (CV-AFS). The Ni/NixB nanoparticles, were synthesized by the chemical reduction of Ni(II) to Ni/NixB. The novel adsorbent was selective to Hg(2+) and CH3Hg(+) species between pH values of 4 - 10. Both of the mercury species were recovered from the adsorbent using 1.0 mol L(-1) hot HNO3 with high efficiency. It was observed that the adsorbent selectively removed Hg(2+) and CH3Hg(+) from the bulk solution in the presence of several competitor ions (As(3+), Sb(3+), Pb(2+), Zn(2+), Cu(2+), Cd(2+) and Fe(3+)) with ≥96% adsorption. The limit of detection (3σ above blank) was found to be 1.8 ng L(-1) with a preconcentration factor of 20. The validation of the method was tested through spike recovery experiments with several water samples (tap and seawater) at μg L(-1) concentration levels, and all recovery values were found to vary between 95 and 105%. PMID:27506713

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-02-01

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

  12. The accuracy of X-ray fluorescence spectrometric determination of Rb and Sr contents in rock sample

    International Nuclear Information System (INIS)

    It is shown that application of the Compton scattering method in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide element contents at an accuracy level +- 1 %

  13. 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.

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

    International Nuclear Information System (INIS)

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

  15. 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%.

  16. 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.

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

    Science.gov (United States)

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

    2009-11-15

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

  18. Study on Arsenic/Selenium Speciation Analysis by a Modified High Sensitive Atomic Fluorescence Spectrometric System%高灵敏度原子荧光光谱系统应用于砷、硒形态分析的研究

    Institute of Scientific and Technical Information of China (English)

    张硕; 弓振斌

    2014-01-01

    将实验室自制的高灵敏度原子荧光光谱系统与色谱分离、在线紫外光前处理装置联用,实现了元素形态的液相色谱分离、在线紫外消解、蒸气发生及原子荧光光谱测定,并以砷、硒两元素为例对系统的分析性能进行研究。样品通过加热混旋提取、离心、过滤,使用反相色谱柱并以5.0 mmol/L磷酸氢二铵缓冲溶液(pH 5.7)-0.5 mmol/L四丁基溴化铵(TBAB)-1%甲醇为流动相进行分离;三价砷(AsO3-3)、二甲基砷( DMA)、一甲基砷( MMA)、五价砷( AsO3-4)可在7 min内进行分离和测定,硒代胱氨酸( SeCys)、硒代蛋氨酸( SeMet)、四价硒( SeO2-3)、六价硒( SeO2-4)的测定约需11 min。在优化实验条件下,方法检出限( DLs,S/N=3)为0.08~0.74μg/L;相对标准偏差( RSD,n=7)为1.4%~7.9%,实际样品的加标回收率为82.5%~116.5%;砷、硒各形态在0.28~40.0μg/L和0.38~80.0μg/L范围内线性良好。建立的联用系统稳定性好、检出限低,可实现样品中低浓度砷、硒形态的准确测定。%A self-mode labs high sensitive atomic fluorescence spectrometric detection system com-bined with liquid chromatography,online ultraviolet photochemical digesting and vapor generation de-vice was established and evaluated. Arsenic and selenium species in various samples were extracted by heating-shaking and centrifugal filtration. All the analytes were separated on a reversed-phase col-umn using mobile phase of 5. 0 mmol/L phosphate buffer(pH 5. 7)-0. 5 mmol/L tetrabutyl ammonium bromide(TBAB)-1% methanol. The separations of AsO3-3 ,DMA,MMA,AsO3-4 and SeCys,SeMet, SeO2-3 ,SeO2-4 were achieved within 7 min and 11 min,respectively. Under the optimized operating con-ditions,the detection limits(DLs,S/N=3)were in the range of 0. 08-0. 74 μg/L,and the relative standard deviations( RSD,n=7 )were 1. 4% -7. 9%. The standard spiked recoveries for real samples

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

    International Nuclear Information System (INIS)

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

  20. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    International Nuclear Information System (INIS)

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  1. 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.

  2. Chromatographic separation and inductively coupled plasma atomic emission spectrometric determination of the rare earth metals contained in terbium

    International Nuclear Information System (INIS)

    The chromatographic separation of rare earth elements (REEs), prior to inductively coupled plasma atomic emission spectrometric (ICP-AES) measurements, using a column packed with 2-ethylexyl hydrogen 2-ethyl-hexylphosphonate (PC-88A)-loaded polymer resin in order to exclude spectral interferences was examined. A favourable separation of trace amounts of metals (La, Nd and Sm) from a large amount of terbium was achieved simply by elution with dilute hydrochloric acid. Trace lanthanum and neodymium in metallic terbium were determined by separation of the analyte ions from the matrix element followed by ICP-AES analysis. (author). 16 refs.; 5 figs.; 2 tabs

  3. X-ray fluorescence spectrometric and optical emission spectographic analysis of thoria in thoriated copper metal powder

    International Nuclear Information System (INIS)

    Two methods, one using the X-ray fluorescence (XRF) spectrometric technique and another using optical emission spectrographic (OES) technique are described for the determination of thoria in the concentration range 0.5-10% in thoriated copper metal powder. The precision of XRF method is superior to OES method but when sample quantity is very small, the OES method is useful. For XRF method, 500 mg sample is mixed with boric acid binding material and converted to a tablet for analysis. For OES method, only 200 mg sample is needed which is glued to the flat ends of two graphite electrodes for excitation by AC arc. The precision obtained in XRF is better than +-1% and in OES it is +-23%. (author)

  4. 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

  5. Analyses of Heavy Metal Contents in the Bulk Atmospheric Aerosols Simultaneously Collected at Okinawa Archipelago, Japan by Using X-ray fluorescence spectrometric method (XRF)

    Science.gov (United States)

    Oshiro, Y.; ITOH, A.; Azechi, S.; Somada, Y.; Handa, D.; Miyagi, Y.; Arakaki, T.; Tanahara, A.

    2012-12-01

    We studied heavy metal contents of bulk atmospheric aerosols using an X-ray fluorescence spectrometric method (XRF). The XRF method enables us to analyze heavy metal contents in the bulk aerosols rapidly without any chemical pretreatments. We used an energy dispersive X-ray fluorescence spectrometer that is compact and portable. We prepared several different amounts of standard reference materials (referred to "SRM", NIES No.28 of Japanese National Institute of Environmental Studies) on quartz filters for calibration curves in two different methods; 1) water-insoluble materials were collected after dispersing SRM in pure water and filtered with the quartz filters ("wet method"), and 2) SRM was dispersed in air in the plastic container and the aerosols were collected by using the low-volume air sampler ("dry method"). Good linear relationships between X-ray intensity and amount of aerosols on the filter were seen in the following 9 metals; Al, K, Ti, V, Fe, Ni, Rb, Ba, and Pb (with wet method) and 12 metals; K, Ti, Fe, Ni, Rb, Ba, Pb, Sr, Ca, Mn, Zn, and Cu (with dry method). Furthermore, we evaluated quantitative responses of XRF method by comparing with the metal contents determined by inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS) after acid-digestion. We then used XRF method to determine heavy metal contents in authentic atmospheric aerosols collected in Okinawa islands, Japan. We simultaneously collected bulk aerosol samples by using identical high-volume air samplers at 3 islands; Cape Hedo Atmospheric Aerosol Monitoring Station (CHAAMS, Okinawa island), Kume island (ca. 160 km south-west of CHAAMS), and Minami-Daitou island (ca. 320 km south-east of CHAAMS). We report and discuss spatial and temporal distribution of heavy metals determined by the XRF method in the bulk atmospheric aerosols collected at the three islands during June 2008 to June 2010, and for CHAAMS during June 2008 to October 2012.

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

    International Nuclear Information System (INIS)

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

  7. Determination of rhenium in molybdenite by X-ray fluorescence. A combined chemical-spectrometric technique

    Science.gov (United States)

    Solt, M.W.; Wahlberg, J.S.; Myers, A.T.

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 ??g of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. ?? 1969.

  8. 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.

  9. Determination of rhenium in molybdenite by X-ray fluorescence: A combined chemical-spectrometric technique.

    Science.gov (United States)

    Solt, M W; Wahlberg, J S; Myers, A T

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 microg of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. PMID:18960464

  10. 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.

  11. Atomic-spectrometric determination of lithium, sodium, potassium and strontium in high-pure scandium

    International Nuclear Information System (INIS)

    Determination of lithium, sodium and potassium in strontium by flame photometry with atomic-absorption spectrophotometer is described. Scandium effect on value of Li, K. Na analytical signal in flame is studied. It is shown, that the base understates analytical signals. Determination of strontium by flame photometry is impossible. Determination of strontium (1x10-13 kg/ml) by atomic-absorption method with electrothermal atomization is possible

  12. 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.

  13. 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.

  14. Characterization of Heavy Metal Contents in the Bulk Atmospheric Aerosols Simultaneously Collected at Three Islands in Okinawa, Japan by X-ray fluorescence spectrometric method (XRF)

    Science.gov (United States)

    Oshiro, Y.; ITOH, A.; Azechi, S.; Somada, Y.; Handa, D.; Miyagi, Y.; Arakaki, T.; Tanahara, A.

    2011-12-01

    We studied heavy metal contents of atmospheric aerosols using an X-ray fluorescence spectrometric method (XRF). The XRF method enables us to analyze heavy metal contents of bulk aerosols rapidly without any chemical pretreatments. We used an energy dispersive X-ray fluorescence spectrometer that is compact and portable. We prepared several different amounts of standard reference materials (NIES No.28) of Japanese National Institute of Environmental Studies on quartz filters for calibration curves. Then, we evaluated quantitative responses of XRF method by comparing with the metal contents determined by inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS) after acid-digestion. Good linear relationships between X-ray intensity and amount of aerosol on filter were seen in the following 10 metals; Al, K, Ti, V, Fe, Ni, Rb, Ba, Pb and As. We then used XRF method to determine heavy metal contents in authentic atmospheric aerosols collected in Okinawa islands, Japan. Okinawa islands, consisting of many small islands, are situated east of Asian continent, and its location in Asian is well suited for studying long-range transport of air pollutants. Also, in Okinawa islands, maritime air mass prevails during summer, while Asian continental air mass dominates during fall, winter, and spring. The maritime air mass data can be seen as background clean air and can be compared with continental air mass which has been affected by anthropogenic activities such as industries and automobiles. Therefore, Okinawa region is suitable area for studying impacts of air pollutants from East Asia. We simultaneously collected bulk aerosol samples by using identical high-volume air samplers at 3 islands; Cape Hedo Atmospheric Aerosol Monitoring Station (CHAAMS, Okinawa island), Kume island (ca. 160 km south-west of CHAAMS), and Minami-Daitou island (ca. 320 km south-east of CHAAMS). We report and discuss spatial and temporal distribution of heavy metals

  15. Single-atom-sensitive fluorescence imaging of ultracold quantum gases

    CERN Document Server

    Bücker, R; Manz, S; Betz, T; Koller, Ch; Plisson, T; Rottmann, J; Schumm, T; Schmiedmayer, J

    2009-01-01

    We present a novel imaging system for ultracold quantum gases in expansion. After release from a confining potential, atoms fall through a sheet of resonant excitation laser light and the emitted fluorescence photons are imaged onto an amplified CCD camera using a high numerical aperture optical system. The imaging system reaches an extraordinary dynamic range, not attainable with conventional absorption imaging. We demonstrate single-atom detection for dilute atomic clouds with high efficiency where at the same time dense Bose-Einstein condensates can be imaged without saturation or distortion. The spatial resolution can reach the sampling limit as given by the 8 microns pixel size in object space. Pulsed operation of the detector allows for slice images and hence a 3D tomography of the measured object. The scheme can easily be implemented for any atomic species and all optical components are situated outside the vacuum system. As a first application we perform thermometry on rubidium Bose-Einstein condensat...

  16. Atomic absorbtion spectrometric determination of platinum, palladium and rhodium in catalysts for automotive exhaust

    International Nuclear Information System (INIS)

    Analytical parameters of the electrothermal atomic absorption spectrometry method have been optimized for determination of platinum, palladium and rhodium in ceramic-supported catalysts for automobile exhaust gas treatment. Two chemical sample preparation methods have been proposed. In order to simplify the sample preparation procedure and to prevent the possible losses of platinum group metals the treatment of the previously ground sample with a mixture of mineral acids is recommended. (authors)

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

    International Nuclear Information System (INIS)

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

  18. 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...

  19. Studies in atomic-fluorescence spectroscopy-V The fluorescence characteristics and determination of antimony.

    Science.gov (United States)

    Dagnall, R M; Thompson, K C; West, T S

    1967-10-01

    Atomic-fluorescence of antimony may be generated in an air-propane flame by nebulizing aqueous solutions of antimony salts whilst irradiating the flame by means of a microwave-excited electrode-less discharge tube operating at 30 W. The strongest fluorescence is exhibited by the (4)S(11 2 ) --> (4)P(1 3 ) 2311 A resonance line and weaker signals are observed at the 2068 and 2176 A resonance lines and at four intercombination lines, at 2598, 2671, 2770 and 2878 A. A process of thermally assisted direct-line fluorescence is postulated to account for the otherwise inexplicable intensity of the 2598 A line emission. Atomic-fluorescence spectroscopy at 2176 A permits the determination of antimony in the range 0.1-120 ppm with a detection limit of 0.05 ppm. With the same equipment and source, the range of measurement for atomic-absorption was 6-120 ppm and the detection limit was 1 ppm. No interferences were observed from 100-fold molar amounts of Cd, Co, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, NH(4), Pb and Zn or from arsenate, chloride, nitrate, phosphate and sulphate. PMID:18960212

  20. 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.

  1. 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.

  2. Microwave plasma atomic emission spectrometric determination of Ca, K and Mg in various cheese varieties.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2016-02-01

    Microwave plasma-atomic emission spectrometry (MP-AES) was used to determine calcium, magnesium and potassium in various Turkish cheese samples. Cheese samples were dried at 100 °C for 2 days and then digested in a mixture of nitric acid/hydrogen peroxide (3:1). Good linearities (R(2) > 0.999) were obtained up to 10 μg mL(-1) of Ca, Mg and K at 445.478 nm, 285.213 nm and 766.491 nm, respectively. The analytes in a certified reference milk powder sample were determined within the uncertainty limits. Moreover, the analytes added to the cheese samples were recovered quantitatively (>90%). All determinations were performed using aqueous standards for calibration. The LOD values for Ca, Mg and K were 0.036 μg mL(-1), 0.012 μg mL(-1) and 0.190 μg mL(-1), respectively. Concentrations of Ca, K and Mg in various types of cheese samples produced in different regions of Turkey were found between 1.03-3.70, 0.242-0.784 and 0.081-0.303 g kg(-1), respectively. PMID:26304350

  3. 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.

  4. Fluorescence detection at the atom shot noise limit for atom interferometry

    CERN Document Server

    Rocco, Emanuele; Valenzuela, Tristan; Boyer, Vincent; Freise, Andreas; Bongs, Kai

    2014-01-01

    Atom interferometers are promising tools for precision measurement with applications ranging from geophysical exploration to tests of the equivalence principle of general relativity, or the detection of gravitational waves. Their optimal sensitivity is ultimately limited by their detection noise. We review resonant and near-resonant methods to detect the atom number of the interferometer outputs and we theoretically analyze the relative influence of various scheme dependent noise sources and the technical challenges affecting the detection. We show that for the typical conditions under which an atom interferometer operates, simultaneous fluorescence detection with a CCD sensor is the optimal imaging scheme. We extract the laser beam parameters such as detuning, intensity, and duration, required for reaching the atom shot noise limit.

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

    International Nuclear Information System (INIS)

    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 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−1 and 1.0 ng l−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−1

  6. 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}.

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

    DEFF Research Database (Denmark)

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

    2010-01-01

    The reliable detection of single quantum particles has revolutionized the field of quantum optics and quantum information processing. For several years, researchers have aspired to extend such detection possibilities to larger-scale, strongly correlated quantum systems 1 , 2 in order to record...... 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...... 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...

  8. Titanium atom detection by resonance fluorescence excited with a nitrogen laser

    International Nuclear Information System (INIS)

    Coincidence of wave lengths of nitrogen laser basing lines and resonance transitions in titanium atom is investigated. It is shown that resonance fluorescence excited by nitrogen laser can be used for absolute titanium atom density measurements. Experiments on titanium atom detection in a vapour cloud formed under irradiation of a titanium target in vacuum by dye laser pulse, are conducted. Fluorescence extinguishing is observed under high evaporation power

  9. 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.

  10. 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.

  11. Energy dispersive x-ray fluorescence spectrometric determination of vanadium, nickel, and iron in petroleum and petroleum residua

    International Nuclear Information System (INIS)

    Trace metals such as vanadium, nickel, and iron in fluid catalytic cracking feedstocks deposit on the catalyst and adversely affect catalyst activity and product yields. Vanadium compounds can also cause damage to furnace linings and corrosion of boiler tubes or gas turbine blades. A rapid and sensitive analytical method is need to detect these metals in feedstocks, products, and residual. In this paper such a method using energy dispersive X-ray fluorescence (EDXRF) spectrometry for determination of vanadium, nickel, and iron in petroleum and petroleum residua is described. In order to eliminate matrix effects, samples containing an internal standard (cobalt) were decomposed by heating with concentrated sulfuric acid and the resulting carbonaceous residua were ashed. X-ray fluorescent spectral intensities of V, Ni, Fe, and Co were measured using established instrumental parameters. Since the Fe Kβ and Co Kα lines overlapped, the slope and the intercept of the ratio of Fe Kα to Fe Kβ intensities from the analysis of ash of several iron standards were used for correction of Co spectral intensities. Sample metal concentrations were determined by comparison of spectral ratios to those of ashed calibration standards

  12. Laser-excitation atomic fluorescence spectroscopy in a helium microwave-induced plasma

    Science.gov (United States)

    Schroeder, Timothy S.

    The focus of this dissertation is to report the first documented coupling of helium microwave induced plasmas (MIPs) to laser excitation atomic fluorescence spectroscopy. The ability to effectively produce intense atomic emission from both metal and nonmetal analytes gives helium microwave induced plasmas a greater flexibility than the more commonly utilized argon inductively coupled plasma (ICP). Originally designed as an element selective detector for non-aqueous chromatography applications at low applied powers (plasma has been applied to aqueous sample determinations at higher applied powers (>500 W). The helium MIP has been shown to be a very powerful analytical atomic spectroscopy tool. The development of the pulsed dye laser offered an improved method of excitation in the field of atomic fluorescence. The use of laser excitation for atomic fluorescence was a logical successor to the conventional excitation methods involving hollow cathode lamps and continuum sources. The highly intense, directional, and monochromatic nature of laser radiation results in an increased population of atomic species in excited electronic states where atomic fluorescence can occur. The application of laser excitation atomic fluorescence to the analysis of metals in a helium microwave induced plasma with ultrasonic sample nebulization was the initial focus of this work. Experimental conditions and results are included for the aqueous characterization of manganese, lead, thallium, and iron in the helium MIP- LEAFS system. These results are compared to previous laser excitation atomic fluorescence experimentation. The effect of matrix interferences on the analytical fluorescence signal was also investigated for each element. The advantage of helium MIPs over argon ICPs in the determination of nonmetals in solution indicates that the helium MIP is an excellent candidate for laser excitation atomic fluorescence experiments involving nonmetals such as chlorine, bromine, iodine, and

  13. Cooperative Fluorescence from a Strongly Driven Dilute Cloud of Atoms

    OpenAIRE

    Ott, Johan Raunkjær; Wubs, Martijn; Lodahl, Peter; Mortensen, N. Asger; Kaiser, R.

    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...

  14. Optical resonance shifts in the fluorescence imaging of thermal and cold Rubidium atomic gases

    CERN Document Server

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

    2016-01-01

    We show that the resonance shifts in fluorescence of a cold gas of rubidium atoms substantially differ from those of thermal atomic ensembles that obey the standard continuous medium electrodynamics. The analysis is based on large-scale microscopic numerical simulations and experimental measurements of the resonance shifts in a steady-state response in light propagation.

  15. Novel laser atomic fluorescence spectrometer for environmental and biomedical analyses of heavy metals

    Science.gov (United States)

    Dergachev, Alex Y.; Mirov, Sergey B.; Pitt, Robert E.; Parmer, Keith D.

    1997-05-01

    We report on the development of a novel experimental set-up using laser atomic fluorescence for detection and concentration measurements of heavy metal atoms for environmental and biomedical analyses. This spectrometer is based on the application of tunable LiF:F2+** and LiF:F2- color center and alexandrite lasers with nonlinear converters for narrowband excitation of atomic fluorescence and the use of gated multichannel CCD detectors for fluorescence measurements. A standard graphite furnace module was used for sample atomization. The laser sources used provide narrowband selective laser excitation continuously tunable in the 200 - 400 nm range and are therefore suitable for resonant excitation of atomic transitions in practically all known heavy metal atoms. In the first experiments, water samples containing Cu, Pb and Fe impurities were studied and detection levels of less than 1 ppb were observed. Comparison of the results of atomic laser fluorescence analysis and traditional atomic absorption spectrometry showed good qualitative agreement between these two methods. It is projected that full optimization of our experimental set up will allow for improved detection levels of several orders of magnitude. Possible optimization and simplification of the spectrometer are discussed in the context of developing a portable instrument for field use.

  16. 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.

  17. 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.

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

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

    2005-06-01

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

  3. Mass spectrometric determination of atomization energies of inorganic molecules and their correlation by empirical models of bonding

    International Nuclear Information System (INIS)

    The application of the Knudsen effusion method combined with mass spectrometry for the measurement of atomization energies of inorganic molecules is described. Recent results with emphasis on molecular metals, intermetallic molecules and metal carbides are presented. The use and limitations of various empirica models of bonding are illustrated by comparing experimental values with those calculated by the various models

  4. Electrothermal atomic absorption spectrometric determination of lithium, sodium, potassium and copper in uranium without preliminary chemical separation

    International Nuclear Information System (INIS)

    Graphite furnace atomization is used for the direct determination of Li (0.25-4 ppm), Na (8-70 ppm), K (20-300 ppm) and Cu (0.5-25 ppm) in uranium dissolved in nitric acid, with relative standard deviations of 4-9%. Only iron seriously depresses the signals from the alkali metals. (Auth.)

  5. 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...

  6. 微波消解-原子荧光光谱法测定宫瘤消片中的砷、镉%Measuring of arsenic and lead in the Gongliuxiao tablets by microwave digestion and atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    运行; 安迎雪; 尤海丹

    2012-01-01

    Objective: To develop a atomic fluorescence spectrometric method for the determination of heavy metals ( As,Cd) in Gongliuxiao. Method:Sample were digested with microwave system,and the As,Gd were directly analyzed by atomic fluorescence spectrometric. Result:For the analyzed heavy metals,the correlative coefficient of the calibration curves was over0. 9992,the recovery was 91. 5% -97. 8% ,RSD was less 5%. Conclusion:The method is convenient and highly sensitive. The method had been applied to the determination of trace heavy metals in traditional Chinese medicine with satisfactory results.%目的:测定宫瘤消片中的砷、镉.方法:采用微波消解的制样方法,利用原子荧光光谱法测定了宫瘤消片中镉、砷微量元素的含量.结果:测得2种元素,标准曲线的r>0.9992,回收率为91.5%~97.8%,RSD <5%.结论:本法快速、准确且灵敏度高,为宫瘤消片中重金属含量测定提供了较好的方法,结果满意.

  7. 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.

  8. 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

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

    OpenAIRE

    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 microscope enables a direct comparison between features observed in the fluorescence microscope and those observed in the images obtained with the AFM, in air or under liquid. The cracks in polymerized La...

  10. Nitrogen atom detection in low-pressure flames by two-photon laser-excited fluorescence

    OpenAIRE

    Bittner, Jürgen; Lawitzki, Annette; Meier, Ulrich; Kohse-Höinghaus, Katharina

    1991-01-01

    Nitrogen atoms have been detected in stoichiometric flat premixed H2/O2/N2 flames at 33 and 96 mbar doped with small amounts of NH3, HCN, and (CN)2 using two-photon laser excitation at 211 nm and fluorescence detection around 870 nm. The shape of the fluorescence intensity profiles versus height above the burner surface is markedly different for the different additives. Using measured quenching rate coefficients and calibrating with the aid of known N-atom concentrations in a discharge flow r...

  11. The stationary resonance fluorescence of a two-level atom in a cat-state field

    Science.gov (United States)

    Tomilin, V. A.; Il'ichov, L. V.

    2016-09-01

    We investigate the resonance fluorescence of a two-level atom placed in non-classical field which is a superposition of Glauber coherent states. The source of this superposition known under the common name of 'Schrödinger cat'-states is explicitly incorporated into the model. This let us to explore the stationary regime. In the strong (multiphoton) field limit the steady-state of the atom+photons system is found. We evaluated the spectrum of the resonance fluorescence. It appears to be one-component in contrast to the case with the classical external field.

  12. 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.

  13. 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.

  14. 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...

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

    International Nuclear Information System (INIS)

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

  16. 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.

  17. 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.

  18. 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…

  19. 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

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

    CERN Document Server

    Jones, Ryan; Olmos, Beatriz

    2016-01-01

    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 smaller than 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 driving limit, we make progress in understanding the signatures of collective behavior in these many-body systems. Furthermore, we clarify the role of disorder 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.

  1. 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.

  2. 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

  3. Fluorescence spectra of atomic ensembles in a magneto-optical trap as an optical lattice

    CERN Document Server

    Yoon, Seokchan; Kang, Sungsam; Kim, Wook-Rae; Kim, Jung-Ryul; An, Kyungwon

    2015-01-01

    We present a study on characteristics of a magneto-optical trap (MOT) as an optical lattice. Fluorescence spectra of atoms trapped in a MOT with a passively phase-stabilized beam configuration have been measured by means of the photon-counting heterodyne spectroscopy. We observe a narrow Rayleigh peak and well-resolved Raman sidebands in the fluorescence spectra which clearly show that the MOT itself behaves as a three-dimensional optical lattice. Optical-lattice-like properties of the phase-stabilized MOT such as vibrational frequencies and lineshapes of Rayleigh peak and Raman sidebands are investigated systematically for various trap conditions.

  4. 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. PMID:26745991

  5. Energy dissipation in matrix-isolated silver atoms: A time-resolved fluorescence study

    Science.gov (United States)

    Wiggenhauser, H.; Schroeder, W.; Kolb, D. M.

    1988-03-01

    The fluorescence from optically excited Ag atoms in Ar, Kr, and Xe matrices has been investigated in a time-resolved synchrotron-radiation study. A detailed energy dissipation model could be established from a systematic analysis of rise and decay times of all the observed fluorescence bands after pulsed excitation into the Ag (4d105p)2P1/2,3/2 levels, and by setting time windows between the excitation pulses in emission and emission-yield spectroscopy. Although the overall wavelength dependence of the decay time follows the λ3 law, the decay time is independent of λ within a given emission band. Finally, the role of energy transfer between Ag atoms and dimers for the evaluation of decay times is briefly addressed.

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

    OpenAIRE

    Spedden, Elise; White, James D.; 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 ganglio...

  7. Simultaneous differential spinning disk fluorescence optical sectioning microscopy and nanomechanical mapping atomic force microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Miranda, Adelaide; De Beule, Pieter A. A., E-mail: pieter.de-beule@inl.int [Applied Nano-Optics Laboratory, International Iberian Nanotechnology Laboratory, Avenida Mestre José Veiga, s/n, 4715-330 Braga (Portugal); Martins, Marco [Nano-ICs Group, International Iberian Nanotechnology Laboratory, Avenida Mestre José Veiga, s/n, 4715-330 Braga (Portugal)

    2015-09-15

    Combined microscopy techniques offer the life science research community a powerful tool to investigate complex biological systems and their interactions. Here, we present a new combined microscopy platform based on fluorescence optical sectioning microscopy through aperture correlation microscopy with a Differential Spinning Disk (DSD) and nanomechanical mapping with an Atomic Force Microscope (AFM). The illumination scheme of the DSD microscope unit, contrary to standard single or multi-point confocal microscopes, provides a time-independent illumination of the AFM cantilever. This enables a distortion-free simultaneous operation of fluorescence optical sectioning microscopy and atomic force microscopy with standard probes. In this context, we discuss sample heating due to AFM cantilever illumination with fluorescence excitation light. Integration of a DSD fluorescence optical sectioning unit with an AFM platform requires mitigation of mechanical noise transfer of the spinning disk. We identify and present two solutions to almost annul this noise in the AFM measurement process. The new combined microscopy platform is applied to the characterization of a DOPC/DOPS (4:1) lipid structures labelled with a lipophilic cationic indocarbocyanine dye deposited on a mica substrate.

  8. Simultaneous differential spinning disk fluorescence optical sectioning microscopy and nanomechanical mapping atomic force microscopy

    International Nuclear Information System (INIS)

    Combined microscopy techniques offer the life science research community a powerful tool to investigate complex biological systems and their interactions. Here, we present a new combined microscopy platform based on fluorescence optical sectioning microscopy through aperture correlation microscopy with a Differential Spinning Disk (DSD) and nanomechanical mapping with an Atomic Force Microscope (AFM). The illumination scheme of the DSD microscope unit, contrary to standard single or multi-point confocal microscopes, provides a time-independent illumination of the AFM cantilever. This enables a distortion-free simultaneous operation of fluorescence optical sectioning microscopy and atomic force microscopy with standard probes. In this context, we discuss sample heating due to AFM cantilever illumination with fluorescence excitation light. Integration of a DSD fluorescence optical sectioning unit with an AFM platform requires mitigation of mechanical noise transfer of the spinning disk. We identify and present two solutions to almost annul this noise in the AFM measurement process. The new combined microscopy platform is applied to the characterization of a DOPC/DOPS (4:1) lipid structures labelled with a lipophilic cationic indocarbocyanine dye deposited on a mica substrate

  9. Plasma jet desorption atomization-atomic fluorescence spectrometry and its application to mercury speciation by coupling with thin layer chromatography.

    Science.gov (United States)

    Liu, Zhifu; Zhu, Zhenli; Zheng, Hongtao; Hu, Shenghong

    2012-12-01

    A novel plasma jet desorption atomization (PJDA) source was developed for atomic fluorescence spectrometry (AFS) and coupled on line with thin layer chromatography (TLC) for mercury speciation. An argon dielectric barrier discharge plasma jet, which is generated inside a 300 μm quartz capillary, interacts directly with the sample being analyzed and is found to desorb and atomize surface mercury species rapidly. The effectiveness of this PJDA surface sampling technique was demonstrated by measuring AFS signals of inorganic Hg(2+), methylmercury (MeHg), and phenylmercury (PhHg) deposited directly on TLC plate. The detection limits of the proposed PJDA-AFS method for inorganic Hg(2+), MeHg, and PhHg were 0.51, 0.29, and 0.34 pg, respectively, and repeatability was 4.7%, 2.2%, and 4.3% for 10 pg Hg(2+), MeHg, and PhHg. The proposed PJDA-AFS was also successfully coupled to TLC for mercury speciation. Under optimized conditions, the measurements of mercury dithizonate (Hg-D), methylmercury dithizonate (MeHg-D), and phenylmercury dithizonate (PhHg-D) could be achieved within 3 min with detection limits as low as 8.7 pg. The combination of TLC with PJDA-AFS provides a simple, cost-effective, relatively high-throughput way for mercury speciation. PMID:23153091

  10. 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.

  11. Commercial Applications of X Ray Spectrometric Techniques

    International Nuclear Information System (INIS)

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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. Fluorescent atom coincidence spectroscopy of extremely neutron-deficient barium isotopes

    International Nuclear Information System (INIS)

    Fluorescent atom coincidence spectroscopy (FACS) has been used to measure the nuclear mean square radii and moments of the extremely neutron-deficient isotopes 120-124Ba. At N=65 an abrupt change in nuclear mean square charge radii is observed which can be understood in terms of the occupation of the spin-orbit partner g7/2 5/2[413] neutron and g9/2 9/2[404] proton orbitals and the consequent enhancement of the n-p interaction. (orig.)

  17. 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)

    Mao, Xuefei; Qi, Yuehan; Huang, Junwei; Liu, Jixin; Chen, Guoying; Na, Xing; Wang, Min; Qian, Yongzhong

    2016-04-01

    A novel dielectric barrier discharge reactor (DBDR) was utilized to trap/release arsenic coupled to hydride generation atomic fluorescence spectrometry (HG-AFS). On the DBD principle, the precise and accurate control of trap/release procedures was fulfilled at ambient temperature, and an analytical method was established for ultratrace arsenic in real samples. Moreover, the effects of voltage, oxygen, hydrogen, and water vapor on trapping and releasing arsenic by DBDR were investigated. For trapping, arsenic could be completely trapped in DBDR at 40 mL/min of O2 input mixed with 600 mL/min Ar carrier gas and 9.2 kV discharge potential; prior to release, the Ar carrier gas input should be changed from the upstream gas liquid separator (GLS) to the downstream GLS and kept for 180 s to eliminate possible water vapor interference; for arsenic release, O2 was replaced by 200 mL/min H2 and discharge potential was adjusted to 9.5 kV. Under optimized conditions, arsenic could be detected as low as 1.0 ng/L with an 8-fold enrichment factor; the linearity of calibration reached R(2) > 0.995 in the 0.05 μg/L-5 μg/L range. The mean spiked recoveries for tap, river, lake, and seawater samples were 98% to 103%; and the measured values of the CRMs including GSB-Z50004-200431, GBW08605, and GBW(E)080390 were in good agreement with the certified values. These findings proved the feasibility of DBDR as an arsenic preconcentration tool for atomic spectrometric instrumentation and arsenic recycling in industrial waste gas discharge. PMID:26976077

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

    International Nuclear Information System (INIS)

    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 SnH4 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.

  19. 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%.

  20. Temperature imaging of turbulent dilute spray flames using two-line atomic fluorescence

    Science.gov (United States)

    Medwell, Paul R.; Masri, Assaad R.; Pham, Phuong X.; Dally, Bassam B.; Nathan, Graham J.

    2014-11-01

    This paper reports the first application of nonlinear excitation regime two-line atomic fluorescence imaging (NTLAF) of indium to measure temperature in turbulent flames of dilute sprays. Indium chloride is dissolved in acetone fuel which is atomised with an ultrasonic nebuliser and supplied with carrier air into a standard piloted burner. It is found that the indium fluorescence signal is not affected by scattering from the droplets or fuel vapour and that no changes to the optical arrangement used with gaseous flames were required. Notwithstanding the lower temperature thresholds of 800 K imposed by the population of excitation species for the NTLAF method and of 1,200 K imposed by the mechanism of releasing gas-phase indium from its salt, the comparisons of conditional and pseudo-unconditional means with thermocouple measurements performed in a range of turbulent spray flames are quite favourable. The NTLAF signal quality deteriorates on the jet centreline at upstream locations and on the lean side of the flame, the former being largely due to insufficient conversion of indium chloride to indium atoms and the latter potentially due to indium oxidation. Nevertheless, the signal-to-noise ratios obtained in the reaction zone regions are good and the results reveal the expected temperature trends in the turbulent spray flames tested here. Further developments are necessary to resolve the mechanism of indium formation and to broaden the temperature range.

  1. Interactions between fluorescence of atomically layered graphene oxide and metallic nanoparticles

    Science.gov (United States)

    Wang, Yu; Li, Shao-Sian; Yeh, Yun-Chieh; Yu, Chen-Chieh; Chen, Hsuen-Li; Li, Feng-Chieh; Chang, Yu-Ming; Chen, Chun-Wei

    2013-01-01

    Graphene oxide (GO) demonstrates interesting photoluminescence (PL) because of its unique heterogeneous atomic structure, which consists of variable sp2- and sp3-bonded carbons. In this study, we report the interaction between the luminescence of GO ranging from a single atomic layer to few-layered thin films and localized surface plasmon resonance (LSPR) from silver nanoparticles (Ag NPs). The photoluminescence of GO in the vicinity of the Ag NPs is enhanced significantly due to the near-field plasmonic effect by coupling electron-hole pairs of GO with oscillating electrons in Ag NPs, leading to an increased PL intensity and a decreased PL decay lifetime. The maxima 30-fold enhancement in PL intensity is obtained with an optimized film thickness of GO, and the luminescence image from a single atomic layer GO sheet is successfully observed with the assistance of the LSPR effect. The results provide an ideal platform for exploring the interactions between the fluorescence of two-dimensional layered materials and the LSPR effect.Graphene oxide (GO) demonstrates interesting photoluminescence (PL) because of its unique heterogeneous atomic structure, which consists of variable sp2- and sp3-bonded carbons. In this study, we report the interaction between the luminescence of GO ranging from a single atomic layer to few-layered thin films and localized surface plasmon resonance (LSPR) from silver nanoparticles (Ag NPs). The photoluminescence of GO in the vicinity of the Ag NPs is enhanced significantly due to the near-field plasmonic effect by coupling electron-hole pairs of GO with oscillating electrons in Ag NPs, leading to an increased PL intensity and a decreased PL decay lifetime. The maxima 30-fold enhancement in PL intensity is obtained with an optimized film thickness of GO, and the luminescence image from a single atomic layer GO sheet is successfully observed with the assistance of the LSPR effect. The results provide an ideal platform for exploring the

  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. 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

  4. Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza, E-mail: luis.claudio@ctmsp.mar.mil.br, E-mail: adriana@ctmsp.mar.mil.br, E-mail: gomide@ctmsp.mar.mil.br, E-mail: ieda@ctmsp.mar.mil.br [Centro Tecnologico da Marinha em Sao Paulo (CEA/CTMSP), Ipero, SP (Brazil). Centro Experimental Aramar

    2013-07-01

    A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

  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. 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...

  7. Method of trivalent chromium concentration determination by atomic spectrometry

    Science.gov (United States)

    Reheulishvili, Aleksandre N.; Tsibakhashvili, Neli Ya.

    2006-12-12

    A method is disclosed for determining the concentration of trivalent chromium Cr(III) in a sample. The addition of perchloric acid has been found to increase the atomic chromium spectrometric signal due to Cr(III), while leaving the signal due to hexavalent chromium Cr(VI) unchanged. This enables determination of the Cr(III) concentration without pre-concentration or pre-separation from chromium of other valences. The Cr(III) concentration may be measured using atomic absorption spectrometry, atomic emission spectrometry or atomic fluorescence spectrometry.

  8. 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.

  9. Time-resolved fluorescence spectroscopy of matrix-isolated silver atoms after pulsed excitation of inner-shell transitions

    Science.gov (United States)

    Hebert, T.; Wiggenhauser, H.; Schriever, U.; Kolb, D. M.

    1990-02-01

    The energy dissipation in matrix-isolated silver atoms after pulsed vacuum ultraviolet (VUV) excitation of 4d-5p transitions has been studied by time-resolved fluorescence spectroscopy. The decay behavior of the various fluorescence bands has been analyzed and a model for the relaxation process proposed within the framework of a two-dimensional configuration-coordinate diagram. If minute quantities of Ag2 are present in the matrix, the analysis requires consideration of energy transfer between silver atoms and dimers.

  10. Probing intra-molecular mechanics of single circularly permuted green fluorescent protein with atomic force microscopy

    International Nuclear Information System (INIS)

    We investigated the mechanical unfolding of single circularly permuted green fluorescent protein (cpGFP) with atomic force microscopy (AFM). The molecule was stretched from its N- and C-termini by an external force causing an elongation of the polypeptide chain up to its full length. The features of the force-extension (F-E) curves were found to depend on the stretching speed. At fast speeds, we detected one peak in the F-E curves before final rupture of the extended molecule, which we interpreted as the unfolding of two terminal halves within cpGFP. We observed several more force peaks in a sawtooth pattern at much slower speeds, and explained the appearance of such force peaks as cooperative unfolding of the hidden sub-structures inside each terminal half

  11. Atomic layer deposition to prevent metal transfer from implants: An X-ray fluorescence study

    Science.gov (United States)

    Bilo, Fabjola; Borgese, Laura; Prost, Josef; Rauwolf, Mirjam; Turyanskaya, Anna; Wobrauschek, Peter; Kregsamer, Peter; Streli, Christina; Pazzaglia, Ugo; Depero, Laura E.

    2015-12-01

    We show that Atomic Layer Deposition is a suitable coating technique to prevent metal diffusion from medical implants. The metal distribution in animal bone tissue with inserted bare and coated Co-Cr alloys was evaluated by means of micro X-ray fluorescence mapping. In the uncoated implant, the migration of Co and Cr particles from the bare alloy in the biological tissues is observed just after one month and the number of particles significantly increases after two months. In contrast, no metal diffusion was detected in the implant coated with TiO2. Instead, a gradient distribution of the metals was found, from the alloy surface going into the tissue. No significant change was detected after two months of aging. As expected, the thicker is the TiO2 layer, the lower is the metal migration.

  12. Velocity and electronic state distributions of sputtered Fe atoms by laser-induced fluorescence spectroscopy

    International Nuclear Information System (INIS)

    Velocity distributions and relative populations in the fine-structure levels of the a5D/sub J/ ground state of Fe atoms, produced by sputtering with 3 keV argon ions, have been investigated by Doppler shifted laser induced fluorescence. The laser system employs a single-mode, scanning ring dye laser, amplified by a sequence of three excimer-pumped flowing-dye cells. Frequency doubling in a KD*P crystal was used to produce high energy (> .5 mJ) pulses of narrowband tunable UV output near 300 nm. Laser power influence on effective velocity bandwidth was investigated. Favorable light-collection geometry minimized distortion of the velocity spectra from apparatus-averaging effects. In impurity flux diagnostic applications in fusion devices, substantial spatial averaging may occur. In the latter case, the narrow velocity bandwidth (70 m/s, transform limit) of the present laser system is particularly useful

  13. 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

  14. 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...

  15. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-05-15

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

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

    International Nuclear Information System (INIS)

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

  18. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Reyes, Mariela N.M.; Cervera, Maria L.; Guardia, Miguel de la, E-mail: m.luisa.cervera@uv.e [University of Valencia, Valencia (Spain). Dept. of Analytical Chemistry

    2011-07-01

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L{sup -1} phosphoric acid, 1 mol L{sup -1} nitric acid, aqua regia, 1 mol L{sup -1} sulfuric acid and 6 mol L{sup -1} hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H{sub 2}SO{sub 4} the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g{sup -1} with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  19. Determination of inorganic species of Sb and Te in cereals by hydride generation atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    A non-chromatographic fast, sensitive and easy method has been developed for the determination of Sb(III), Sb(V), Te(IV) and Te(VI) in cereal samples. The procedure is based on ultrasound assisted extraction and determination by hydride generation atomic fluorescence spectrometry (HG AFS). Preliminary studies were made in order to get the best extraction efficiency using 1 mol L-1 phosphoric acid, 1 mol L-1 nitric acid, aqua regia, 1 mol L-1 sulfuric acid and 6 mol L-1 hydrochloric acid. The extraction with aqua regia showed a clear interconversion of the species during the process, being H2SO4 the best extractant with efficiencies greater than 90% from the total content of Sb and Te quantified previously and without species interconversion. This point was checked by recovery experiments at different spiked levels. The method provided limits of detection values from 0.1 to 0.5 ng g-1 with relative standard deviation values from 5.4 to 9.2% of 10 independent analysis of samples containing few ng g-1 of Sb and Te species. (author)

  20. Determination of cadmium in water samples by fast pyrolysis-chemical vapor generation atomic fluorescence spectrometry

    Science.gov (United States)

    Zhang, Jingya; Fang, Jinliang; Duan, Xuchuan

    2016-08-01

    A pyrolysis-vapor generation procedure to determine cadmium by atomic fluorescence spectrometry has been established. Under fast pyrolysis, cadmium ion can be reduced to volatile cadmium species by sodium formate. The presence of thiourea enhanced the efficiency of cadmium vapor generation and eliminated the interference of copper. The possible mechanism of vapor generation of cadmium was discussed. The optimization of the parameters for pyrolysis-chemical vapor generation, including pyrolysis temperature, amount of sodium formate, concentration of hydrochloric acid, and carrier argon flow rate were carried out. Under the optimized conditions, the absolute and concentration detection limits were 0.38 ng and 2.2 ng ml- 1, respectively, assuming that 0.17 ml of sample was injected. The generation efficiency of was 28-37%. The method was successfully applied to determine trace amounts of cadmium in two certified reference materials of Environmental Water (GSB07-1185-2000 and GSBZ 50009-88). The results were in good agreement with the certified reference values.

  1. 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%.

  2. 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...

  3. 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.)

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

    Directory of Open Access Journals (Sweden)

    Farid Shakerian

    2013-01-01

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

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

    Science.gov (United States)

    Conway, J.; Gogna, G. S.; Gaman, C.; Turner, M. M.; Daniels, S.

    2016-08-01

    Atomic oxygen number density [O] is measured in an air atmospheric pressure plasma jet (APPJ) using two-photon absorption laser induced fluorescence (TALIF). Gas flow is fixed at 8 slpm, the RF power coupled into the plasma jet varied between 5 W and 20 W, and the resulting changes in atomic oxygen density measured. Photolysis of molecular oxygen is employed to allow in situ calibration of the TALIF system. During calibration, O2 photo-dissociation and two-photon excitation of the resulting oxygen atoms are achieved within the same laser pulse. The atomic oxygen density produced by photolysis is time varying and spatially non-uniform which needs to be corrected for to calibrate the TALIF system for measurement of atomic oxygen density in plasma. Knowledge of the laser pulse intensity I 0(t), wavelength, and focal spot size allows correction factors to be determined using a rate equation model. Atomic oxygen is used for calibration and measurement, so the laser intensity can be increased outside the TALIF quadratic laser power dependence region without affecting the calibration reliability as the laser power dependence will still be the same for both. The atomic O density results obtained are not directly benchmarked against other known density measurement techniques. The results show that the plasma jet atomic oxygen content increases as the RF power coupled into the plasma increases.

  6. 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。

  7. 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.

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

    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

  10. 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.

  11. Combining atomic force-fluorescence microscopy with a stretching device for analyzing mechanotransduction processes in living cells.

    Science.gov (United States)

    Hecht, E; Knittel, P; Felder, E; Dietl, P; Mizaikoff, B; Kranz, C

    2012-11-21

    Mechanical forces affect biological systems in their natural environment in a widespread manner. Mechanical stress may either stimulate cells or even induce pathological processes. Cells sensing mechanical stress usually respond to such stressors with proliferation or differentiation. Hence, for in vitro studies, the ability to impose a controlled mechanical stress on cells combined with appropriate analytical tools providing an immediate answer is essential to understand such fundamental processes. Here, we present a novel uniaxial motorized cell stretching device that has been integrated into a combined fluorescence microscope (FM)-atomic force microscope (AFM) system, thereby enabling high-resolution topographic and fluorescent live cell imaging. This unique tool allows the investigation of mechanotransduction processes, as the cells may be exposed to deliberately controlled mechanical stress while simultaneously facilitating fluorescence imaging and AFM studies. The developed stretching device allows applying reproducible uniaxial strain from physiologically relevant to hyperphysiological levels to cultured cells grown on elastic polydimethylsiloxane (PDMS) membranes. Exemplarily, stretching experiments are shown for transfected squamous cell carcinoma cells (SCC-25) expressing fluorescent labeled cytokeratin, whereby fluorescence imaging and simultaneously performed AFM measurements reveal the cytokeratin (CSK) network. Topographical changes and mechanical characteristics such as elasticity changes were determined via AFM while the cells were exposed to mechanical stress. By applying a cell deformation of approx. 20%, changes in the Young's modulus of the cytoskeletal network due to stretching of the cells were observed. Consequently, integrating a stretching device into the combined atomic force-fluorescence microscope provides a unique tool for dynamically analyzing structural remodeling and mechanical properties in mechanically stressed cells. PMID:22977882

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

  15. 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.

  16. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-11-21

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

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

    Science.gov (United States)

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

    2014-11-01

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

  19. 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.

  20. Highly uniform holographic microtrap arrays for single atom trapping using a feedback optimization of in-trap fluorescence measurements.

    Science.gov (United States)

    Tamura, Hikaru; Unakami, Tomoyuki; He, Jun; Miyamoto, Yoko; Nakagawa, Ken'ichi

    2016-04-18

    We report on the novel optimization method to realize highly uniform microtrap arrays for single atom trapping with a spatial light modulator (SLM). This method consists of two iterative feedback loops with the measurements of both diffracted light intensities and in-trap fluorescence intensities from each microtrap. By applying this method to the single 87Rb atom trapping, we can reduce the variance of trap depths from 20.8% to 1.7% for 4 × 4 square arrays and less than 4% for various arrays with up to 62 sites. The detection error of individual single atoms is also reduced from 1.7% to 0.0054% on average. PMID:27137252

  1. 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.

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

    Science.gov (United States)

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

  7. 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.

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

    Science.gov (United States)

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

    2010-01-01

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

  9. 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.

  10. 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...

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

    Science.gov (United States)

    Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

    2009-06-30

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

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

    Science.gov (United States)

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

    2009-10-01

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

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. 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).

  18. 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,…

  19. Direct visualization of triplex DNA molecular dynamics by fluorescence resonance energy transfer and atomic force microscopy measurements

    Science.gov (United States)

    Chang, Chia-Ching; Lin, Po-Yen; Chen, Yen-Fu; Chang, Chia-Seng; Kan, Lou-Sing

    2007-11-01

    We have detected the dynamics of 17-mer DNA triplex dissociation mechanism at the molecular level. Fluorescence resonance energy transfer (FRET) was used as an indicator of intermolecular interaction in nanometer range, whereas atomic force microscopy (AFM) was employed to address single molecule with sub-angstrom precision. The maximum rupture force of DNA triplex was found at pH 4.65, consistent with macroscopic observations. These results indicated that the FRET together with an AFM detection system could be used to reveal the DNA triplex interaction in nanometer scale unambiguously.

  20. Analysis of Local Structures around Ni Atoms Doped in ZnO-Based Diluted Magnetic Semiconductors by Fluorescence EXAFS

    Institute of Scientific and Technical Information of China (English)

    LI Bin-Bin; XIU Xiang-Qian; ZHANG Rong; TAO Zhi-Kuo; CHEN Lin; XIE Zi-Li; ZHENG You-Dou; HE Bo

    2006-01-01

    @@ Zn1-xNixO (x = 0.001, 0.01, 0.02, 0.05 and 0.20) powders are prepared by sol-gel method. An extended x-ray absorption fine structure technique (EXAFS) for the Ni K-edge is employed to probe the local structures around Ni atoms doped in ZnO powders by fluorescence mode. The near edge EXAFS of the samples does not change in the range of Ni concentration from x = 0.001 to 0.05, which is consistent with the results of x-ray diffraction of the samples. The simulation results for the first shell EXAFS signals indicated that Ni atoms are substituted in Zn sites.

  1. 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

  2. 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.

  3. 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...

  4. 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).

  5. Fluorescence properties in a single driven four-level atomic system

    Institute of Scientific and Technical Information of China (English)

    Jiang Xiang-Qian; Lǖ Zhi-Wei; Zhang Bing; Sun Xiu-Dong

    2010-01-01

    The spontaneous emission decay dynamics of a tripod configuration four-level atom driven by a single laser field is studied.Under different initial conditions,we discuss the effects of quantum interference and detuning of external driving field on atomic spontaneous emission properties.For the larger detuning,the interesting phenomena of the spectral line narrowing are found which stem from the contribution of external driving field.

  6. 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.

  7. 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.

  8. Fluorescence excitation spectra of jet-cooled complexes of carbazole and mono-atomic alcohols

    International Nuclear Information System (INIS)

    Fluorescence excitation spectra of jet-cooled complexes of carbazole and one molecule of methyl, deuterated methyl, ethyl and propyl (propanol-1 and propanol-2) alcohols are analyzed. Shifts of the fluorescence excitation spectra of complexes relative to the frequency of a pure electron transition of unbound carbazole are determined. They are formed owing to the hydrogen bonds of the N-H groups of carbazole with the OH-group of alcohols. The frequencies of stretching vibrations of hydrogen groups with various alcohols vary within the range 150-157 cm-1, whereas for the deformation ones the frequencies fall in the interval 21-22.9 cm-1. The belonging of complexes to rotational conformers is determined through the shape of the rotational contours of bands of their pure electronic and electron-vibration transitions. Equilibrium configurations of complexes in the ground state are calculated (authors)

  9. Determination of Selenium in Marine Aquatic Products by Hydride Generation-atomic Fluorescence Spectrometry (HG-AFS)

    Institute of Scientific and Technical Information of China (English)

    ZHANG Zhaohui; GAO Xin; Tashiro Yuri; Hiroo Ogawa

    2005-01-01

    A method for the analysis of selenium in marine aquatic products by HG-AFS has been investigated. The method is based on the reduction of inorganic selenium to volatile SeH2 which is bubbled out by carrier gas of pure argon, and then swept to Ar-H2 flame quarts atomizer to measure its fluorescence intensity. The hydride generation, transportation, atomization and some instrumental parameters were studied by a kind of orthogonal design. The optimum conditions selected are as follows: reactive acidity, 20% HC1; the amount of NaBH4, 4.9mL; gas flow of argon, 600mLmin-1; atomizing temperature, 200 ℃; negative high voltage, -300V; light current, 100 mA; integral time, 7s. The detection limit of the presented method is 0.072μgL-1 for selenium. The calibration curve shows a satisfactory line inthe concentration range from 0.000 to1.000μgL-1 Se. The recovery is 95.8%-102.2%.

  10. 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)

  11. Determination of air Stannum in Workplace by L-cysteine and Atomic Fluorescence Spectrometry%工作场所空气中锡的L-半胱氨酸-原子荧光测定法

    Institute of Scientific and Technical Information of China (English)

    牛晓梅

    2011-01-01

    [Objective]To determine the air stannum in workplaces by hydride generation-atomic fluorescence spectrometry, with the existence of L-cysteine. [ Methods ] After digested by hydrochloric acid, the samples were determined by atomic fluorescence spectrometer with 2% hydrochloric acid as carrier liquid. [ Results] The range of measurement was 5. 0 ~ 200.0 μg/L, the RSD was 2.15% ~ 3.40%, the recoveries ranged from 92. 5% ~ 103.5% ,and the detection limits of this method was 0. 71 μg/L [ Conclusion] Due to the presence of L-cysteine, the hydride generation conditions are improved, the spectrometric signal is enhanced, and the acidity of solution is reduced. In addition, the interferences of the metal elements are significantly inhibited. The method is suitable for determination of air stannum in workplace.%目的 利用氢化物发生-原子荧光光谱法,在L-半胱氨酸存在的情况下,测定工作场所空气中的锡.方法 样品经盐酸消解,用2%盐酸溶液做载流,原子荧光分光光度计进行测定.结果 方法的测定范围为5.0~200.0 μg/L,相对标准偏差为2.15%~3.40%,回收率为92.5%~103.5%,检出限为0.71 μg/L.结论 由于L-半胱氨酸的存在,改善了氢化物发生条件,增敏光谱测定信号,降低了溶液的酸度,金属离子的干扰显著地得到了抑制,适用于工作场所空气中锡的测定.

  12. L-半胱氨酸-原子荧光法测定食品中的硒%Determination of selenium in food by L-Cysteine atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    牛晓梅

    2011-01-01

    目的:利用氢化物发生-原子荧光光谱法,在L-半胱氨酸存在下,测定食品中的硒.方法:样品经酸加热消化后,用2%盐酸溶液做载流,原子荧光分光光度计进行测定.结果:方法的测定范围为10.0μg/L~50.0μg/L,相对标准偏差为0.70%~1.90%,回收率为93.0%~101.0%,检出限为0.051μg/L.结论:由于L-半胱氨酸的存在,改善了氢化物发生条件,增敏光谱测定信号,降低了溶液的酸度,金属离子的干扰显著地得到了抑制,适用于食品中硒的测定.%Objective: In this paper, we give a method for determination of selenium in food by hydride generation -atomic fluorescence spectrometry in the presence of L- Cysteine.Methods: Using 2% hydrochloric acid as carrier liquid, the samples were determined by atomic fluorescence spectrometry after been digested by heating in acid.Results: The measurement range of this method was 10.0 μg/L ~ 50.0 μg/L, the RSD 0.7 % ~ 1.9%, the recoveries were in the range of 93.0% ~ 101.0% and the detection limits of this method were found to be 0.051 μg/L.Conclusion: In the presence of L - Cysteine, the hydride generation conditions were improved, the spectrometric signal was enhanced, and the acidity of solution was reduced.In addition, the interferences of the metal elements were significantly inhibited.The method can be used to determine seleium in food.

  13. 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.

  14. Fluorescence spectroscopy in the nanosecond range for matrix-isolated Cu atoms and dimers

    Science.gov (United States)

    Wiggenhauser, H.; Kolb, D. M.; Rotermund, H. H.; Schrittenlacher, W.; Schroeder, W.

    1985-11-01

    Synchrotron radiation in the single-bunch mode was employed to study time-resolved emission from Cu atoms and dimers isolated in a Ne matrix. The decay time of the matrix-related emission at 3.5 eV for Cu in Ne after excitation of the 4s → 4p resonance transition was determined as 6.9±0.3 ns, while excitation into higher-lying 3d → 4p transitions resulted in a much slower decay of the 3.5 eV emission. From analysis of rise and decay times, a detailed diagram for energy dissipation in matrix-isolated Cu atoms has been derived. The B → X (Σ u → Σ g) emission of Cu 2 in Ne has a first-order decay time of about 10 ns.

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

    Science.gov (United States)

    Lu, Weifang; Ou, Yiyu; Jokubavicius, Valdas; Fadil, Ahmed; Syväjärvi, Mikael; Petersen, Paul Michael; Ou, Haiyan

    2016-07-01

    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 for TiO2 deposition, a three-step cleaning procedure was introduced after RIE etching. The morphology of anatase TiO2 indicates that the nano-textured substrate has a much higher surface nucleated grain density than a flat substrate at the beginning of the deposition process. The corresponding reflectance increases with TiO2 thickness due to increased surface diffuse reflection. The passivation effect of ALD TiO2 thin film on the nano-textured fluorescent 6H-SiC sample was also investigated and a PL intensity improvement of 8.05% was obtained due to the surface passivation.

  16. Electric field strength measurements in a megavolt vacuum diode using laser induced fluorescence of an atomic beam

    International Nuclear Information System (INIS)

    A combined technique of an atomic beam probing and laser-induced fluorescence spectroscopy (LIFABS) is applied for measuring of local electric field in a 1 MV, 100 kJ, 4 μsec electron diode. Laser-produced lithium beam is stepwise excited by two resonant wide-band laser beams. Stark-splitted spontaneous emission from n=4 level is detected with a polychromator. Time dependence of the electric field was inferred from splitting of the 460.3 nm lithium line. The electric field strength F grows during a pulse from 160 to 260 kV/cm in the center of a 6 cm gap. By comparing calculated and experimental F-values, expansion of the emission boundaries of the cathode and anode plasmas was reconstructed

  17. Two-Photon Laser-Induced Fluorescence O and N Atoms for the Study of Heterogeneous Catalysis in a Diffusion Reactor

    Science.gov (United States)

    Pallix, Joan B.; Copeland, Richard A.; Arnold, James O. (Technical Monitor)

    1995-01-01

    Advanced laser-based diagnostics have been developed to examine catalytic effects and atom/surface interactions on thermal protection materials. This study establishes the feasibility of using laser-induced fluorescence for detection of O and N atom loss in a diffusion tube to measure surface catalytic activity. The experimental apparatus is versatile in that it allows fluorescence detection to be used for measuring species selective recombination coefficients as well as diffusion tube and microwave discharge diagnostics. Many of the potential sources of error in measuring atom recombination coefficients by this method have been identified and taken into account. These include scattered light, detector saturation, sample surface cleanliness, reactor design, gas pressure and composition, and selectivity of the laser probe. Recombination coefficients and their associated errors are reported for N and O atoms on a quartz surface at room temperature.

  18. 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.

  19. 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.

  20. High-Sensitivity In situ Fluorescence Imaging of Ytterbium Atoms in a Two-Dimensional Optical Lattice with Dual Optical Molasses

    Science.gov (United States)

    Shibata, Kosuke; Yamamoto, Ryuta; Takahashi, Yoshiro

    2014-01-01

    We developed a dual molasses technique which enabled us to perform high-sensitivity in situ fluorescence imaging of ytterbium (Yb) atoms in a two-dimensional optical lattice prepared in a thin glass cell. This technique successfully combines two different kinds of optical molasses for Yb atoms, that is, the one using the 1S0-1P1 transition which provides high-resolution in the in situ fluorescence imaging and the other using the 1S0-3P1 transition for cooling the atoms in the optical lattice. We performed in situ imaging of 174Yb atoms and could observe a Moiré pattern with a period of about 6 µm produced by the molasses beam with 556 nm and the optical lattice with 532 nm, which implies that the temperature was kept below the lattice depth during the fluorescence imaging. The number of photons per atom is estimated to be enough for single atom detection with our imaging system. This result is quite promising for the realization of an Yb quantum gas microscope.

  1. 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.

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

    International Nuclear Information System (INIS)

    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 N2 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 N2 discharge pulse is estimated to be 2.9 - 9.8 × 1013 atoms and the energy efficiency of atomic nitrogen production is estimated to be about 1.8 - 6.1 × 1016 atoms/J. The energy efficiency of atomic nitrogen production in N2 discharge is constant against the discharge energy, while that in N2/O2 discharge increases with discharge energy. In the N2/O2 discharge, two-step process of N2 dissociation plays significant role for atomic nitrogen production.

  3. 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.

  4. Ultra-trace determination of methylmercuy in seafood by atomic fluorescence spectrometry coupled with electrochemical cold vapor generation.

    Science.gov (United States)

    Zu, Wenchuan; Wang, Zhenghao

    2016-03-01

    A homemade electrochemical flow cell was adopted for the determination of methylmercury. The cold vapor of mercury atoms was generated from the surface of glassycarbon cathode through the method of electrolytic reduction and detected by atomic fluorescence spectroscopy subsequently. The operating conditions were optimized with 2 ng mL(-1) methylmercury standard solution. The caliberation curve was favorably linear when the concentrations of standard HgCH3(+) solutions were in the range of 0.2-5 ng mL(-1)(as Hg). Under the optimized conditions, the limit of detection (LOD) for methylmercury was 1.88×10(-3)ng mL(-1) and the precision evaluated by relative standard deviation was 2.0% for six times 2 ng mL(-1) standard solution replicates. The terminal analytical results of seafood samples, available from local market, showed that the methylmercury content ranged within 3.7-45.8 ng g(-1). The recoveries for methylmercury spiked samples were found to be in the range of 87.6-103.6% and the relative standard deviations below 5% (n=6) were acquired, which showed this method was feasible for real sample analysis. PMID:26615576

  5. Determination of Mercury in Aqueous and Geologic Materials by Continuous Flow-Cold Vapor-Atomic Fluorescence Spectrometry (CVAFS)

    Science.gov (United States)

    Hageman, Philip L.

    2007-01-01

    New methods for the determination of total mercury in geologic materials and dissolved mercury in aqueous samples have been developed that will replace the methods currently (2006) in use. The new methods eliminate the use of sodium dichromate (Na2Cr2O7 ?2H2O) as an oxidizer and preservative and significantly lower the detection limit for geologic and aqueous samples. The new methods also update instrumentation from the traditional use of cold vapor-atomic absorption spectrometry to cold vapor-atomic fluorescence spectrometry. At the same time, the new digestion procedures for geologic materials use the same size test tubes, and the same aluminum heating block and hot plate as required by the current methods. New procedures for collecting and processing of aqueous samples use the same procedures that are currently (2006) in use except that the samples are now preserved with concentrated hydrochloric acid/bromine monochloride instead of sodium dichromate/nitric acid. Both the 'old' and new methods have the same analyst productivity rates. These similarities should permit easy migration to the new methods. Analysis of geologic and aqueous reference standards using the new methods show that these procedures provide mercury recoveries that are as good as or better than the previously used methods.

  6. 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.

  7. 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.

  8. Mass Spectrometric Analysis of Water-soluble Gold Nanoclusters

    International Nuclear Information System (INIS)

    Batches of water-soluble gold nanoclusters of nominal 2.0 or 3.5-nm diameter were prepared to evaluate particle size determinations by a number of techniques such as transmission electron microscopy or atomic force microscopy and to validate estimates derived by mass spectrometric analysis using matrix-assisted laser desorption ionization (MALDI). Good agreement was found and MALDI lends itself to analyses even in the presence of aggregates

  9. 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. PMID:22970588

  10. 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.

  11. 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%.

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

    Science.gov (United States)

    Zhou, Qingxiang; Zhao, Na; Xie, Guohong

    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(-1) (r(2) = 0.9990). The precision was 2.12% (RSD, n = 7) and the detection limit was 0.95 ng L(-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%. PMID:21398026

  13. Ultrasensitive determination of mercury in human saliva by atomic fluorescence spectrometry based on solidified floating organic drop microextraction

    International Nuclear Information System (INIS)

    We report on a new, rapid and simple method for the determination of ultra-trace quantities of mercury ion in human saliva. It is based on solidified floating organic drop microextraction and detection by cold vapor atomic fluorescence spectrometry (CV-AFS). Mercury ion was complexed with diethyldithiocarbamate, and the hydrophobic complex was then extracted into fine droplets of 1-undecanol. By cooling in an ice bath after extraction, the droplets in solution solidify to form a single ball floating on the surface of solution. The solidified micro drop containing the mercury complex was then transferred for determination by CV-AFS. The effects of pH value, concentration of chelating reagent, quantity of 1-undecanol, sample volume, equilibration temperature and time were investigated. Under the optimum conditions, the preconcentration of a 25-mL sample is accomplished with an enrichment factor of 182. The limit of detection is 2.5 ng L-1. The relative standard deviation for seven replicate determinations at 0.1 ng mL-1 level is 4.1%. The method was applied to the determination of mercury in saliva samples collected from four volunteers. Two volunteers having dental amalgam fillings had 0.4 ng mL-1 mercury in their saliva, whereas mercury was not detectable in the saliva of two volunteers who had no dental fillings. (author)

  14. Determination of methyl mercury by aqueous phase Eehylation, followed by gas chromatographic separation with cold vapor atomic fluorescence detection

    Science.gov (United States)

    De Wild, John F.; Olsen, Mark L.; Olund, Shane D.

    2002-01-01

    A recent national sampling of streams in the United States revealed low methyl mercury concentrations in surface waters. The resulting median and mean concentrations, calculated from 104 samples, were 0.06 nanograms per liter (ng/L) and 0.15 ng/L, respectively. This level of methyl mercury in surface water in the United States has created a need for analytical techniques capable of detecting sub-nanogram per liter concentrations. In an attempt to create a U.S. Geological Survey approved method, the Wisconsin District Mercury Laboratory has adapted a distillation/ethylation/ gas-phase separation method with cold vapor atomic fluorescence spectroscopy detection for the determination of methyl mercury in filtered and unfiltered waters. This method is described in this report. Based on multiple analyses of surface water and ground-water samples, a method detection limit of 0.04 ng/L was established. Precision and accuracy were evaluated for the method using both spiked and unspiked ground-water and surface-water samples. The percent relative standard deviations ranged from 10.2 to 15.6 for all analyses at all concentrations. Average recoveries obtained for the spiked matrices ranged from 88.8 to 117 percent. The precision and accuracy ranges are within the acceptable method-performance limits. Considering the demonstrated detection limit, precision, and accuracy, the method is an effective means to quantify methyl mercury in waters at or below environmentally relevant concentrations

  15. 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.

  16. 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.

  17. 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。

  18. 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.

  19. 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.

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

    International Nuclear Information System (INIS)

    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

  1. 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.

  2. 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.

  3. 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.

  4. Temperature imaging in low-pressure flames using diode laser two-line atomic fluorescence employing a novel indium seeding technique

    Science.gov (United States)

    Borggren, Jesper; Burns, Iain S.; Sahlberg, Anna-Lena; Aldén, Marcus; Li, Zhongshan

    2016-03-01

    The use of diode lasers for spatially resolved temperature imaging is demonstrated in low-pressure premixed methane-air flames using two-line atomic fluorescence of seeded indium atoms. This work features the advantages of using compact diode lasers as the excitation sources with the benefits of two-dimensional planar imaging, which is normally only performed with high-power pulsed lasers. A versatile and reliable seeding technique with minimal impact on flame properties is used to introduce indium atoms into the combustion environment for a wide range of flame equivalence ratios. A spatial resolution of around 210 µm for this calibration-free thermometry technique is achieved for three equivalence ratios at a pressure of 50 mbar in a laminar flat flame.

  5. Thermal ionization mass spectrometric study of U-Pu-O system

    International Nuclear Information System (INIS)

    First inference from a thermal ionization mass spectrometric study of samples corresponding to the ternary U-Pu-O system, especially if high surface ionization temperatures are employed, is likely to be at variance with that from equilibrium vaporization thermodynamic studies, that the atomic species U and Pu dominate the vapor phase

  6. Removal of Chromophore-proximal Polar Atoms Decreases Water Content and Increases Fluorescence in a Near Infrared Phytofluor

    Directory of Open Access Journals (Sweden)

    Heli eLehtivuori

    2015-11-01

    Full Text Available Genetically encoded fluorescent markers have revolutionized cell and molecular biology due to their biological compatibility, controllable spatiotemporal expression, and photostability. To achieve in vivo imaging in whole animals, longer excitation wavelength probes are needed due to the superior ability of near infrared light to penetrate tissues unimpeded by absorbance from biomolecules or autofluorescence of water. Derived from near infrared-absorbing bacteriophytochromes, phytofluors are engineered to fluoresce in this region of the electromagnetic spectrum, although high quantum yield remains an elusive goal. An invariant aspartate residue is of utmost importance for photoconversion in native phytochromes, presumably due to the proximity of its backbone carbonyl to the pyrrole ring nitrogens of the biliverdin (BV chromophore as well as the size and charge of the side chain. We hypothesized that the polar interaction network formed by the charged side chain may contribute to the decay of the excited state via proton transfer. Thus, we chose to further probe the role of this amino acid by removing all possibility for polar interactions with its carboxylate side chain by incorporating leucine instead. The resultant fluorescent protein, WiPhy2, maintains BV binding, monomeric status, and long maximum excitation wavelength while minimizing undesirable protoporphyrin IXα binding in cells. A crystal structure and time-resolved fluorescence spectroscopy reveal that water near the BV chromophore is excluded and thus validate our hypothesis that removal of polar interactions leads to enhanced fluorescence by increasing the lifetime of the excited state. This new phytofluor maintains its fluorescent properties over a broad pH range and does not suffer from photobleaching. WiPhy2 achieves the best compromise to date between high fluorescence quantum yield and long illumination wavelength in this class of fluorescent proteins.

  7. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-08-01

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

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

    International Nuclear Information System (INIS)

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

  10. Nanodimentional Aggregates In Organic Monolayers Studied With Atomic Force Microscopy (AFM) And Fluorescence Lifetime Imaging Microscopy (FLIM)

    Science.gov (United States)

    Ivanov, George R.; Burov, Julian

    2007-04-01

    Organic monolayers from a fluorescently labeled phospholipid (DPPE-NBD) were deposited on solid supports under special conditions that form stable nanometer wide bilayers cylinders that protrude from the monolayer. This molecule was frequently used in sensor applications due to its sensitivity to environment changes. The proposed configuration should provide both fast response times (ultra thin film) and increased sensitivity (greatly increased surface area). AFM can clearly distinguish between the different phases. The height difference between the solid-expanded and the liquid-expanded phase was measured to be 1.4 nm while the bilayer thickness was 5.6 nm. The solid domains show a 20 % decrease in fluorescence lifetime in comparison to the monolayer as measured by FLIM. This difference in lifetimes is explained in the model of fluorescence self quenching in the solid phase due to the molecules being closer to each other.

  11. Nanoscale orientation and lateral organization of chimeric metal-binding green fluorescent protein on lipid membrane determined by epifluorescence and atomic force microscopy

    International Nuclear Information System (INIS)

    Epifluorescence microscopy as well as atomic force microscopy was successfully applied to explore the orientation and lateral organization of a group of chimeric green fluorescent proteins (GFPs) on lipid membrane. Incorporation of the chimeric GFP carrying Cd-binding region (His6CdBP4GFP) to the fluid phase of DPPC monolayer resulted in a strong fluorescence intensity at the air-water interface. Meanwhile, non-specific adsorption of the GFP having hexahistidine (His6GFP) led to the perturbation of the protein structure in which very low fluorescence was observed. Specific binding of both of the chimeric GFPs to immobilized zinc ions underneath the metal-chelating lipid membrane was revealed. This specific binding could be reversibly controlled by addition of metal ions or metal chelator. Binding of the chimeric GFPs to the metal-chelating lipid membrane was proven to be the end-on orientation while the side-on adsorption was contrarily noted in the absence of metal ions. Increase of lateral mobility owing to the fluidization effect on the chelating lipid membrane subsequently facilitated crystal formation. All these findings have opened up a potential approach for a specific orientation of immobilization of protein at the membrane interface. This could have accounted for a better opportunity of sensor development

  12. 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.

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

  15. 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.

  16. 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

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

    International Nuclear Information System (INIS)

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

  18. 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...

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

    Zachariadis, G A; Rosenberg, E

    2009-04-30

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

  1. In Situ Synchrotron Based X-ray Fluorescence and Scattering Measurements During Atomic Layer Deposition: Initial Growth of HfO2 on Si and Ge Substrates

    Energy Technology Data Exchange (ETDEWEB)

    K Devloo-Casier; J Dendooven; K Ludwig; G Lekens; J DHaen; C Detavernier

    2011-12-31

    The initial growth of HfO{sub 2} was studied by means of synchrotron based in situ x-ray fluorescence (XRF) and grazing incidence small angle x-ray scattering (GISAXS). HfO{sub 2} was deposited by atomic layer deposition (ALD) using tetrakis(ethylmethylamino)hafnium and H{sub 2}O on both oxidized and H-terminated Si and Ge surfaces. XRF quantifies the amount of deposited material during each ALD cycle and shows an inhibition period on H-terminated substrates. No inhibition period is observed on oxidized substrates. The evolution of film roughness was monitored using GISAXS. A correlation is found between the inhibition period and the onset of surface roughness.

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

    Science.gov (United States)

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

    2006-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Wu Hong [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Department of Chemistry, Xuzhou Normal University, Xuzhou 221116 (China); Jin Yan [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Han Weiying [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Miao, Qiang [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China); Bi Shuping [School of Chemistry and Chemical Engineering, State Key Laboratory of Coordination Chemistry and Key Laboratory of MOE for Life Science, Nanjing University, Nanjing 210093 (China)]. E-mail: bisp@nju.edu.cn

    2006-07-15

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

  4. 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.

  5. 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.

  6. Mass spectrometric analysis of isotope effects in bioconversion of benzene to cyclohexanone

    Science.gov (United States)

    Nam, In-Hyun; Murugesan, Kumarasamy; Kim, Young-Mo; Yang, In-Hee; Chang, Yoon-Seok

    2006-06-01

    Pseudomonas veronii strain PH-03 has been shown to convert benzene to cyclohexanone through phenol. Mass spectrometry results revealed that unusual isotopic effects have been occurred in the transformation product, cyclohexanone. The isotopic composition was strongly depends on the compound specific hydrogen or oxygen source. The exchange of labile deuterium atoms has been investigated through electrospray ionization liquid chromatography mass spectrometry. The mass spectrometric analysis of biotransformation products enabled the proposal of a corresponding bioconversion pathway.

  7. 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 ...

  8. Gamma spectrometric assessment of nuclear fuel

    Science.gov (United States)

    Krištof, Edvard; Pregl, Gvido

    1990-12-01

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

  9. [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

  10. [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

  11. In situ preparation and fluorescence quenching properties of polythiophene/ZnO nanocrystals hybrids through atom-transfer radical polymerization and hydrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Peng Xiaoming; Zhang Lin [Department of Chemistry, Nanchang University, Xuefu Road 999, Nanchang 330031 (China); Institute of Polymers/Institute for Advanced study, Nanchang University, Xuefu Road 999, Nanchang 330031 (China); Chen Yiwang, E-mail: ywchen@ncu.edu.cn [Department of Chemistry, Nanchang University, Xuefu Road 999, Nanchang 330031 (China); Institute of Polymers/Institute for Advanced study, Nanchang University, Xuefu Road 999, Nanchang 330031 (China); Li Fan, E-mail: lfan@ncu.edu.cn [Institute of Polymers/Institute for Advanced study, Nanchang University, Xuefu Road 999, Nanchang 330031 (China); Zhou Weihua [Institute of Polymers/Institute for Advanced study, Nanchang University, Xuefu Road 999, Nanchang 330031 (China)

    2010-02-15

    In this paper, a new approach for in situ preparing nanocomposites of conjugated polymers (CPs) and semiconductor nanocrystals was developed. Polythiophene grafted poly(zinc methacrylate) (PTh-g-PZMA) copolymer was synthesized by atom-transfer radical polymerization (ATRP) of zinc methacrylate (ZMA) initiated from the macroinitiator poly(2,5-(3-(bromoisopropyl-carbonyl-oxymethylene) thiophene)) (PTh-Br) with pendant initiator groups. Subsequently, the polythiophene grafted poly(methacrylate)/ZnO (PTh-g-PMA/ZnO) hybrid heterojunction nanocomposites were successfully prepared by in situ hydrolysis of PTh-g-PZMA casting films in alkaline aqueous solution. The structures of PTh-Br, PTh-g-PZMA and PTh-g-PMA/ZnO were confirmed by the proton nuclear magnetic resonance ({sup 1}H NMR) spectra, Fourier transform infrared (FTIR) spectra and X-ray photoelectron spectroscopy (XPS). The morphologies of PTh-g-PMA/ZnO films prepared for different hydrolysis time were observed in the cross-sections by scanning electron microscope (SEM). The SEM images revealed that ZnO nanocrystals were uniformly dispersed in polymers without any aggregation and the appearances of ZnO nanocrystals changed from nanoparticles to nanorods with the hydrolysis treatment time increasing. The optical properties of these nanocomposites were studied by ultraviolet-visible (UV-vis) absorption and fluorescence spectroscopy. UV-vis absorption spectroscopy showed that the adsorption band of PTh-g-PMA/ZnO hybrids was broader than that of PTh-Br, implying that the existence of ZnO nanocrystals increased the optical absorption region of hybrids. The photoluminescence (PL) spectra of the hybrids showed that fluorescence quenching occurred in PTh-g-PMA/ZnO blends and a maximum of 85% of the fluorescence intensity quenched in the PTh-g-PMA/ZnO obtained from treatment in NaOH aqueous solution for 2 h, which revealed the existence of photo-induced charge transfer between the polythiophene chains and ZnO. These results

  12. 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.

  13. 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.

  14. Interaction analysis of chimeric metal-binding green fluorescent protein and artificial solid-supported lipid membrane by quartz crystal microbalance and atomic force microscopy

    International Nuclear Information System (INIS)

    Non-specific adsorption and specific interaction between a chimeric green fluorescent protein (GFP) carrying metal-binding region and the immobilized zinc ions on artificial solid-supported lipid membranes was investigated using the quartz crystal microbalance technique and the atomic force microscopy (AFM). Supported lipid bilayer, composed of octanethiol and 1,2-dipalmitoyl-sn-glycero-3-phosphocholine/1,2-dioleoyl-sn-glycero-3-[N- (5-amino-1-carboxypentyl iminodiacetic acid)succinyl] (NTA-DOGS)-Zn2+, was formed on the gold electrode of quartz resonator (5 MHz). Binding of the chimeric GFP to zinc ions resulted in a rapid decrease of resonance frequency. Reversibility of the process was demonstrated via the removal of metal ions by EDTA. Nanoscale structural orientation of the chimeric GFP on the membrane was imaged by AFM. Association constant of the specific binding to metal ions was 2- to 3-fold higher than that of the non-specific adsorption, which was caused by the fluidization effect of the metal-chelating lipid molecules as well as the steric hindrance effect. This infers a possibility for a further development of biofunctionalized membrane. However, maximization is needed in order to attain closer advancement to a membrane-based sensor device

  15. Determination of As(III) and As(V) in soils using sequential extraction combined with flow injection hydride generation atomic fluorescence detection

    International Nuclear Information System (INIS)

    An analytical procedure for determination of As(III) and As(V) in soils using sequential extraction combined with flow injection (FI) hydride generation atomic fluorescence spectrometry (HG-AFS) was presented. The soils were sequentially extracted by water, 0.6 mol l-1 KH2PO4 solution, 1% (v/v) HCl solution and 1% (w/v) NaOH solution. The arsenite (As(III)) in extract was analyzed by HG-AFS in the medium of 0.1 mol l-1 citric acid solution, then the total arsenic in extract was determined by HG-AFS using on-line reduction of arsenate with L-cysteine. The concentration of arsenate (As(V)) was calculated by the difference. The optimum conditions of extraction and determination were studied in detail. The detection limit (3σ) for As(III) and As(V) were 0.11 and 0.07 μg l-1, respectively. The relative standard deviation (R.S.D.) was 1.43% (n=11) at the 10 μg l-1 As level. The method was applied in the determination of As(III) and As(V) of real soils and the recoveries of As(III) and As(V) were in the range of 89.3-118 and 80.4-111%, respectively

  16. 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.

  17. 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.)

  18. 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. PMID:26988526

  19. 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.

  20. Application of Graphene as a Sorbent for the Preconcentration and Determination of Trace Amounts of Mercury in Water Samples by Hydride Generation Atomic Fluorescence Spectrometry

    International Nuclear Information System (INIS)

    The potential of graphene as a solid-phase extraction adsorbent for the separation and preconcentration of mercury (Hg) was investigated. Hg2+ was found to be quantitatively adsorbed onto graphene within pH 6.0-8.0, and then completely eluted with 4.0 mL of nitric acid/methanol (1:1, v/v) solution at a flow rate of 2.0 mL min-1. A new method using a microcolumn packed with graphene as a sorbent was developed for the preconcentration of trace amount of Hg2+ prior to its determination by hydride generation atomic fluorescence spectrometry. Under the optimum experimental conditions, the detection limit of this method for Hg2+ was 5.0 ng L /sup -1/, with an enrichment factor of 15.0, and the relative standard deviation was 3.5 percentage at the 1.0 μg L-1 Hg /sup 2+/ level. The method was then applied for the determination of trace amount of Hg /sup 2/+ in water samples with satisfactory results. (author)

  1. 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.

  2. Determination of Lead in Kelp by Atomic Fluorescence Spectrometry%氢化物发生原子荧光法测定海带中铅含量

    Institute of Scientific and Technical Information of China (English)

    姜桥; 陈雷; 娄喜山

    2011-01-01

    [ Objective]The aim was to seek a more suitable method in determining the lead of the kelp. [Method] The sample of former process was conducted using the microwave digestion method and the lead of the kelp was determined using the atomic fluorescence spectrometry. [ Result] The detection limit was 0.085 2 μg/L, and RSD was below 10%, the recovery rate was between 89.1% and 107.2%. [ Conclusion] The method was simple,fast,accurate and low pollution to the environment. It was a satisfying result for the determination of lead.%[目的]为检测海带中铅寻找更适合的方法.[方法]采用微波消解法进行样品前处理,用氢化物发生原子荧光光谱法检测海带中的铅.[结果]铅的最低检出限为0.085 2 μg/L,方法的相对标准偏差小于10%,回收率为89.1%~107.2%.[结论]该法简单,快速,灵敏度高,对环境污染轻,用于海带中铅的检测获得令人满意的结果.

  3. 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.

  4. 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.

  5. 原子荧光法测定生活饮用水中砷的含量%Determination of arsenic content in drinking water using atomic fluorescence method

    Institute of Scientific and Technical Information of China (English)

    徐胜

    2015-01-01

    介绍了原子荧光法的原理,论述了采用原子荧光法测定生活饮用水中的砷含量的实验主要仪器、试剂及仪器的工作参数,并对主要的实验步骤进行了详细分析,提出了一些实验注意事项,以供参考。%This paper introduced the principle of atomic fluorescence method,discussed the working parameters of main experiment instrument, reagent and instrument determination of arsenic content in drinking water by atomic fluorescence method,and analyzed in detail the main test steps,put forward some matters needing attention in the test,for reference.

  6. 原子荧光分光光度法检测人尿中锡%Detection of tin in human urine by atomic fluorescence spectrophotometry

    Institute of Scientific and Technical Information of China (English)

    郭晓婧; 郭嘉明; 梁嘉斌; 刘移民

    2016-01-01

    Objective To establish a method for determination of urinary tin by atomic fluorescence spectrophotometry . Methods The graphite digestion instrument was used to digest 2.50 mL urinary sample with 1.50 mL concentrated nitric acid, hydrochloric acid (volume fraction 4.00%) was added to a total constant volume of 10.00 mL.After 2.50 mL of thiocarbamide-ascorbic acid (mass concentration 100 g/L) was added, hydrochloric acid (volume fraction 4.00%) was added to a total constant volume of 25.00 mL ( equivalent to urinary sample was diluted 10 times) , 1.00 mL of the sample was collected and detected by atomic fluorescence spectrophotometry .Results The good linear relationship was shown in the range of 4.00-200.00 μg/L with a correlation coefficient of 0.999 5.The limit of detection was 0.20 μg/L.The recovery rates ranged from 100.20%to 100.84%.The within-run relative standard deviation ( RSD) and between-run RSD were 0.11%-2.01%and 1.37%-5.58%, respectively .The samples can be stored for 7 days under the temperature of 4 ℃.Conclusion This method has the advantages of high sensitivity , precision and convenient operation , which is suitable for the daily determination of urinary tin in human .%目的:建立尿中锡的原子荧光分光光度测定方法。方法取2.50 mL尿样加入1.50 mL浓硝酸后,用石墨消解仪消化,以体积分数为4.00%的盐酸溶液定容至10.00 mL,加入质量浓度为100 g/L的硫脲-抗坏血酸2.50 mL,以体积分数为4.00%的盐酸溶液定容至25.00 mL(相当于稀释尿样10倍)后,取1.00 mL样品采用原子荧光光度法进行测定。结果尿中锡在质量浓度为4.00~200.00μg/L 范围内线性关系良好,相关系数为0.9995;方法检出限为0.20μg/L,加标回收率为100.20%~100.84%,批内相对标准偏差( RSD)为0.11%~2.01%,批间RSD为1.37%~5.58%;样品在4℃条件下可保存7 d。结论本方法灵敏

  7. Uncertainty Assessment of Hydride Generation - Atomic Fluorescence Spectrometry Measurements of Bismuth in Cathode Copper%原子荧光光谱法测定铜精矿中铋的不确定度

    Institute of Scientific and Technical Information of China (English)

    傅宇; 陈红

    2015-01-01

    Based on requirement of national standard GB/T601-2002, Hydride generation-atomic fluorescence spectrometry measurements of uncertainty chemical analysis, this article reviewed the concentration uncertainty of hydride generation-atomic fluorescence spectrometry measurements of bismuth in copper concentrate, mainly introduced the sample solution weighing, constant volume, single mark pipettes, atomic fluorescence spectrometer, sample uniformity, dissolution treatment and working curve simulate and other aspects, and concluded that the combination and expiation was uncertainty.%根据国标氢化物发生——原子荧光光谱法(GB/T601-2002)对化学分析测量的不确定度的要求,对氢化物发生——原子荧光光谱法测定铜精矿中铋含量的不确定度分量进行了评定,主要从样品称量、试液定容、单标线移液管、原子荧光光谱仪、样品的均匀性、溶解处理及工作曲线的线性拟合等方面进行评定,并评定出合成不确定度、扩展不确定度。

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

    International Nuclear Information System (INIS)

    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−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 (Hg2+, CH3Hg+, C2H5Hg+, and C6H5Hg+). 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−1 for CH3Hg+, 13 ng L−1 for Hg2+, 34 ng L−1 for C2H5Hg+ and 30 ng L−1 for C6H5Hg+ for 24 h DGT accumulation at 25 °C

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

    International Nuclear Information System (INIS)

    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 HgII. •Each measure requires less than 5 min with a LOD of 3 ng mL−1 (as mercury). •Hg concentration in commercial ophthalmic solutions ranges between 7.5 and 59.0 μg mL−1. -- Abstract: We developed a flow injection (FI) method for the determination of thiomersal (sodium ethylmercurithiosalicylate, C9H9HgNaO2S) 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 NaBH4 solution, and AFS detection in an Ar/H2 miniaturized flame. The method was linear in the 0.01–2 μg mL−1 range, with a LOD of 0.003 μg mL−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−1

  10. Development of a non-chromatographic method for the speciation analysis of inorganic antimony in mushroom samples by hydride generation atomic fluorescence spectrometry

    Science.gov (United States)

    Sousa Ferreira, Hadla; Costa Ferreira, Sergio Luis; Cervera, M. Luisa; de la Guardia, Miguel

    2009-06-01

    A simple and sensitive method has been developed for the direct determination of toxic species of antimony in mushroom samples by hydride generation atomic fluorescence spectrometry (HG AFS). The determination of Sb(III) and Sb(V) was based on the efficiency of hydride generation employing NaBH 4, with and without a previous KI reduction, using proportional equations corresponding to the two different measurement conditions. The extraction efficiency of total antimony and the stability of Sb(III) and Sb(V) in different extraction media (nitric, sulfuric, hydrochloric, acetic acid, methanol and ethanol) were evaluated. Results demonstrated that, based on the extraction yield and the stability of extracts, 0.5 mol L - 1 H 2SO 4 proved to be the best extracting solution for the speciation analysis of antimony in mushroom samples. The limits of detection of the developed methodology were 0.6 and 1.1 ng g - 1 for Sb(III) and Sb(V), respectively. The relative standard derivation was 3.8% (14.7 ng g - 1 ) for Sb(V) and 5.1% (4.6 ng g - 1 ) for Sb(III). The recovery values obtained for Sb(III) and Sb(V) varied from 94 to 106% and from 98 to 105%, respectively. The method has been applied to determine Sb(III), Sb(V) and total Sb in five different mushroom samples; the Sb(III) content varied from 4.6 to 11.4 ng g - 1 and Sb(V) from 14.7 to 21.2 ng g - 1 . The accuracy of the method was confirmed by the analysis of a certified reference material of tomato leaves.

  11. 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.

  12. 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}.

  13. 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.

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

    International Nuclear Information System (INIS)

    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−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

  15. 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

    2016-03-01

    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. PMID:26717850

  16. Efficient generation of volatile species for cadmium analysis in seafood and rice samples by a modified chemical vapor generation system coupled with atomic fluorescence spectrometry

    International Nuclear Information System (INIS)

    Highlights: • We develop a modified chemical vapor generation method coupled with AFS for the determination of cadmium. • The response of Cd could be increased at least four-fold compared to conventional thiourea and Co(II) system. • A simple mixing sequences experiment is designed to study the reaction mechanism. • The interference of transition metal ions can be easily eliminated by adding DDTC. • The method is successfully applied in seafood samples and rice samples. - Abstract: A vapor generation procedure to determine Cd by atomic fluorescence spectrometry (AFS) has been established. Volatile species of Cd are generated by following reaction of acidified sample containing Fe(II) and L-cysteine (Cys) with sodium tetrahydroborate (NaBH4). The presence of 5 mg L−1 Fe(II) and 0.05% m/v Cys improves the efficiency of Cd vapor generation substantially about four-fold compared with conventional thiourea and Co(II) system. Three experiments with different mixing sequences and reaction times are designed to study the reaction mechanism. The results document that the stability of Cd(II)–Cys complexes is better than Cys–THB complexes (THB means NaBH4) while the Cys–THB complexes have more contribution to improve the Cd vapor generation efficiency than Cd(II)–Cys complexes. Meanwhile, the adding of Fe(II) can catalyze the Cd vapor generation. Under the optimized conditions, the detection limit of Cd is 0.012 μg L−1; relative standard deviations vary between 0.8% and 5.5% for replicate measurements of the standard solution. In the presence of 0.01% DDTC, Cu(II), Pb(II) and Zn(II) have no significant influence up to 5 mg L−1, 10 mg L−1and 10 mg L−1, respectively. The accuracy of the method is verified through analysis of the certificated reference materials and the proposed method has been applied in the determination of Cd in seafood and rice samples

  17. Efficient generation of volatile species for cadmium analysis in seafood and rice samples by a modified chemical vapor generation system coupled with atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Xin-an, E-mail: 13087641@qq.com; Chi, Miao-bin, E-mail: 1161306667@qq.com; Wang, Qing-qing, E-mail: wangqq8812@163.com; Zhang, Wang-bing, E-mail: ahutwbzh@163.com

    2015-04-15

    Highlights: • We develop a modified chemical vapor generation method coupled with AFS for the determination of cadmium. • The response of Cd could be increased at least four-fold compared to conventional thiourea and Co(II) system. • A simple mixing sequences experiment is designed to study the reaction mechanism. • The interference of transition metal ions can be easily eliminated by adding DDTC. • The method is successfully applied in seafood samples and rice samples. - Abstract: A vapor generation procedure to determine Cd by atomic fluorescence spectrometry (AFS) has been established. Volatile species of Cd are generated by following reaction of acidified sample containing Fe(II) and L-cysteine (Cys) with sodium tetrahydroborate (NaBH{sub 4}). The presence of 5 mg L{sup −1} Fe(II) and 0.05% m/v Cys improves the efficiency of Cd vapor generation substantially about four-fold compared with conventional thiourea and Co(II) system. Three experiments with different mixing sequences and reaction times are designed to study the reaction mechanism. The results document that the stability of Cd(II)–Cys complexes is better than Cys–THB complexes (THB means NaBH{sub 4}) while the Cys–THB complexes have more contribution to improve the Cd vapor generation efficiency than Cd(II)–Cys complexes. Meanwhile, the adding of Fe(II) can catalyze the Cd vapor generation. Under the optimized conditions, the detection limit of Cd is 0.012 μg L{sup −1}; relative standard deviations vary between 0.8% and 5.5% for replicate measurements of the standard solution. In the presence of 0.01% DDTC, Cu(II), Pb(II) and Zn(II) have no significant influence up to 5 mg L{sup −1}, 10 mg L{sup −1}and 10 mg L{sup −1}, respectively. The accuracy of the method is verified through analysis of the certificated reference materials and the proposed method has been applied in the determination of Cd in seafood and rice samples.

  18. 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

  19. Multisyringe flow injection lab-on-valve systems coupled to hydride generation atomic fluorescence spectrometry for on-line bead-injection preconcentration and determination of total inorganic arsenic in environmental waters

    DEFF Research Database (Denmark)

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

    In this work, the third generation of flow injection analysis, that is, the so-called micro-Lab-on-Valve (LOV) approach, is hyphenated for the first time to atomic fluorescence spectrometry (AFS) for the separation, preconcentration and monitoring of hydride forming elements. A multisyringe flowing...... before loading into the multisyringe flow system. The flow system facilitates on-column reduction with no need for application of programmable stopped-flow. Yet, the high electrolyte concentrations and extreme pH conditions for elution prevents the sorbent to be re-used, so that maximum benefit can...

  20. 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.

  1. 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.

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

    Science.gov (United States)

    Burguera, José Luis; Burguera, Marcela

    2011-01-15

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

  3. Determination of Arsenic, Mercury and Barium in herbarium mount paper using dynamic ultrasound-assisted extraction prior to atomic fluorescence and absorption spectrometry

    OpenAIRE

    Lummas, S.; Ruiz-Jimenez, J.; Luque de Castro, M.D.; Colston, Belinda; Gonzalez-Rodriguez, Jose; B. Chen; W. Corns

    2011-01-01

    A dynamic ultrasound-assisted extraction method using Atomic Absorption and Atomic Flourescence spectrometers as detectors was developed to analyse mercury, arsenic and barium from herbarium mount paper originating from the herbarium collection of the National Museum of Wales. The variables influencing extraction were optimised by a multivariate approach. The optimal conditions were found to be 1% HNO3 extractant solution used at a flow rate of 1 mL min-1. The duty cycle and amplitude of the ...

  4. Determination of Mercury, Lead and Arsenic in Mainstream Smoke of Cigarette by Atomic Fluorescence Spectroscopy%原子荧光法测定卷烟主流烟气中的汞·砷·铅

    Institute of Scientific and Technical Information of China (English)

    孔维松; 汤丹俞; 曾晓鹰; 者为; 施红林; 张峻松

    2009-01-01

    A new method for the determination of mercury, lead and arsenic in cigarette smoke by using atomic fluorescence spectroscopy was studied.The mainstream cigarette smoke was collected by cambridge filter, and mercury, lead and arsenic were collected with 2% hydrochloric acid ultrasonic leaching filter.The mercury, lead and arsenic in digest were determined by atomic fluorescence spectroscopy.Under the optimum determination conditions, the standard relative standard deviations are 2.8%-3.2% and the recoveries are 91%-95%.%研究了用原子荧光法测定卷烟主流烟气中的汞、砷、铅.结果表明,卷烟主流烟气用剑桥滤片捕集,用2%盐酸超声波浸取滤片上捕集的汞、砷、铅,然后用原子荧光法测定,方法相对标准偏差为2.8%~3.2%,标准回收率为91%~95%.

  5. Mass spectrometry based approach for identification and characterisation of fluorescent proteins from marine organisms

    DEFF Research Database (Denmark)

    Wojdyla, Katarzyna Iwona; Rogowska-Wrzesinska, Adelina; Wrzesinski, Krzysztof;

    2011-01-01

    We present here a new analytical strategy for identification and characterisation of fluorescent proteins from marine organisms. By applying basic proteomics tools it is possible to screen large sample collections for fluorescent proteins of desired characteristics prior to gene cloning. Our...... methodology which includes isolation, spectral characterisation, stability testing, gel-based separation and mass spectrometric identification was optimised on samples collected during the Danish Galathea 3 expedition. Four corals of the Fungia, Sarcophyton and Acropora species emitting green fluorescence...... were tested. Each of the fluorescent extracts behaves differently under denaturing conditions but complete fluorescence loss was not observed. Optimised electrophoretic conditions yielded effective separation of active fluorescent proteins in both 1DE and 2DE. Mass spectrometric analysis...

  6. Mass spectrometry based approach for identification and characterisation of fluorescent proteins from marine organisms

    DEFF Research Database (Denmark)

    Wojdyla, Katarzyna; Rogowska-Wrzesinska, Adelina; Wrzesinski, Krzysztof;

    2011-01-01

    We present here a new analytical strategy for identification and characterisation of fluorescent proteins from marine organisms. By applying basic proteomics tools it is possible to screen large sample collections for fluorescent proteins of desired characteristics prior to gene cloning. Our...... methodology which includes isolation, spectral characterisation, stability testing, gel-based separation and mass spectrometric identification was optimised on samples collected during the Danish Galathea 3 expedition. Four corals of the Fungia, Sarcophyton and Acropora species emitting green fluorescence...... were tested. Each of the fluorescent extracts behaves differently under denaturing conditions but complete fluorescence loss was not observed. Optimised electrophoretic conditions yielded effective separation of active fluorescent proteins in both 1DE and 2DE. Mass spectrometric analysis of the...

  7. Study on laser atomic spectroscopy

    International Nuclear Information System (INIS)

    Electric discharge type atomic vaporizer is developed for the spectroscopic study on actinide elements. Laser induced fluorescence study on actinide elements is performed by using this high temperature type atomizer. For the effective photoionization of elements, copper vapor laser pumped dye laser and electron beam heating type atomic vaporizer are built and their characteristics are measured. In addition, resonance ionization mass spectroscopic analysis for lead sample as well as laser induced fluorescence study on uranium sample in solution phase is made. (Author)

  8. 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)

  9. 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.

  10. 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.

  11. 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。

  12. 浅析原子荧光光谱法同时测定饮用水中砷和汞%Simultaneous Testing of Arsenic and Mercury in Water with Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    段利丽

    2011-01-01

    采用双道原子荧光光度计同时测定饮用水中砷和汞,并进行各种测定条件的试验与研究。结果表明,该方法简单、准确,用于饮用水中砷、汞元素的同时测定具有较好的可行性和适用性。%Arsenic and mercury in water are tested with the dual-channel atomic fluorescence spectrometer in various conditions.The result shows that its easy,precise,feasible and applicable in testing arsenic and mercury in drinking water.

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

    DEFF Research Database (Denmark)

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

    2006-01-01

    In this work, the third generation of flow injection analysis, that is, the so-called micro-Lab-on-Valve (μLOV) approach, is proposed for the first time for the separation, preconcentration and monitoring of metalloids as hyphenated with atomic fluorescence spectrometry (AFS). This was made...... feasible by interfacing the micromachined LOV-module with AFS by a multisyringe flowing stream network for on-line post column derivatization of the eluate aimed at the generation of hydride species. The potential of this new hyphenated technique for environmental assays was ascertained via...... quantified by AFS. The flow system facilitates on-column reduction of the retained arsenic with no need for application of programmable stopped-flow. Yet, the high concentration of reductant and extreme pH conditions for elution hinder the sorbent to be re-used due to the gradual deactivation...

  14. 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).

  15. 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

    International Nuclear Information System (INIS)

    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. - 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

  16. Determination of trace mercury in surface water by atomic fluorescence spectrometry%原子荧光光度法测定地表水中的痕量汞

    Institute of Scientific and Technical Information of China (English)

    潘腊青; 章维维; 池怡; 周姗

    2013-01-01

    以硫酸-高锰酸钾加热消解水样,低浓度硼氢化钾作为还原剂,运用 A FS -9230双道原子荧光光度计,采用顺序注射-冷蒸气发生-原子荧光光谱法,测定地表水中的痕量汞。检出限为0.012μg/L ,回收率为90%~110%,RSD小于10.0%,该法具有灵敏度高,精密度好,干扰少和操作简单方便等优点,同时对方法的质量控制进行了探讨。%Heating and digestion of water samples by sulfuric acid and potassium permanganate ,low concentration potassium borohydride as the reducing agent ,using AFS-9230 double-channel atomic fluo-rescence spectrometry ,determination of trace mercury in surface water with sequential injection-cold vapor generation-atomic fluorescence spectrometry was carried out. The detection limit is 0.012μg/L ,the rate of recovery is 90%-110% ,RSD<10.0%. The advantages of the method are of high sensitivity ,good preci-sion ,less interference ,simple and convenient operation. At the same time ,the aspect of quality control w as discussed.

  17. 氢化物原子荧光光谱法测定铜精矿及铜矿石中砷的研究%Determination of arsenic in copper concentrate and copper ore by hydride atomic fluorescent spectrometry

    Institute of Scientific and Technical Information of China (English)

    胡郁

    2012-01-01

    By removing the disturbance of determined arsenic with the atomic fluorescent spectrometry,which by copper ion and other metal ion in copper concentrate and copper ore,to build a suited dissolution method,and to choose the optimization condition,to overcome the shortage of general atomic fluorescent spectrometry dissolved the sample.The detection limit of the method is 1μg/g.This method is applied to three national standard samples(level one) to detect the content of arsenic.The detected values and recommended ones are consistent.Therefore,the method is feasible to test the content of arsenic in high copper concentrate samples.%通过对铜精矿及铜矿石中大量铜离子等多种金属离子对原子荧光光谱法测定砷干扰的消除,建立一种适合的溶样方法,选择了最佳的分析条件,克服了普通原子荧光法溶解样品的不足,本方法测定砷的检出限为1μg/g。本方法测定了3个国家一级标准物质中砷的含量,测定值与推荐值吻合,确定方法适合铜含量比较高的样品中砷含量的测定。

  18. 原子荧光光谱法测定不同产地油莎豆中重金属含量%Determination of Heavy Metal Content in Cyperus Esculentus from Different Habitats by Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    朱圣芳; 田丽萍; 张天义; 薛琳

    2012-01-01

    目的 测定不同产地油莎豆中重金属含量.方法 采用原子荧光光谱法测定油莎豆中Pb、Cd、As、Hg的含量.结果 不同产地油莎豆中重金属含量存在一定差异,但均远低于《药用植物及制剂进出口绿色行业标准》(2001)中重金属的限量标准,符合标准规定.结论 原子荧光光谱法快速、简便、准确,油莎豆中重金属含量的测定可为油莎豆的质量评价提供参考依据.%OBJECTIVE To determine the content of heavy metal in Cyperus esculentus from different producing areas. METHODS The content of As, Hg, Pb, and Cd in Cyperus esculentus were determined by atomic fluorescence spectrometry. RESULTS There was a certain difference of heavy metal content in Cyperus esculentus from different producing areas, but all heavy metal contents were far below the Green Trade Standards of Importing and Exporting Medicinal Plants and Preparations (2001). The quality was in line with the standard requirements. CONCLUSION Atomic fluorescence spectrometry was rapid, simple and accurate, while the determination of heavy metal in Cyperus esculentus could provide reference for the quality evaluation of Cyperus esculentus.

  19. A comparative study on total reflection X-ray fluorescence determination of low atomic number elements in air, helium and vacuum atmospheres using different excitation sources

    International Nuclear Information System (INIS)

    A comparison of trace element determinations of low atomic number (Z) elements Na, Mg, Al, P, K and Ca in air, helium and vacuum atmospheres using W Lβ1, Mo Kα and Cr Kα excitations has been made. For Mo Kα and W Lβ1 excitations a Si (Li) detector with beryllium window was used and measurements were performed in air and helium atmospheres. For Cr Kα excitation, a Si (Li) detector with an ultra thin polymer window (UTW) was used and measurements were made in vacuum and air atmospheres. The sensitivities of the elemental X-ray lines were determined using TXRF spectra of standard solutions and processing them by IAEA QXAS program. The elemental concentrations of the elements in other solutions were determined using their TXRF spectra and pre-determined sensitivity values. The study suggests that, using the above experimental set up, Mo Kα excitation is not suited for trace determination of low atomic number element. Excitation by WLβ1 and helium atmosphere, the spectrometer can be used for the determination of elements with Z = 15 (P) and above with fairly good detection limits whereas Cr Kα excitation with ultra thin polymer window and vacuum atmosphere is good for the elements having Z = 11 (Na) and above. The detection limits using this set up vary from 7048 pg for Na to 83 pg for Ti. - Highlights: • TXRF conditions are optimized for low atomic number (Z) element determinations. • Mo Kα with Be window detector can be used for elements with Z ≥ 20 (K). • W Lβ1 with Be window detector can be used for elements with Z ≥ 15 (P). • Cr Kα, UTW detector and vacuum atmosphere are suitable for elements with Z ≥ 11 (Na). • For the elements with Z ≥ 11 (Na), a separate study is needed

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

    International Nuclear Information System (INIS)

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

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

    International Nuclear Information System (INIS)

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

  2. Fluorescent silk cocoon creating fluorescent diatom using a “Water glass-fluorophore ferry”

    Science.gov (United States)

    Kusurkar, Tejas S.; Tandon, Ishita; Sethy, Niroj Kumar; Bhargava, Kalpana; Sarkar, Sabyasachi; Singh, Sushil Kumar; Das, Mainak

    2013-11-01

    Fluorophores are ubiquitous in nature. Naturally occurring fluorophores are exceptionally stable and have high quantum yield. Several natural systems have acquired fluorescent signature due to the presence of these fluorophores. Systematic attempt to harvest these fluorophores from natural systems could reap rich commercial benefit to bio-imaging industry. Silk cocoon biomaterial is one such example of natural system, which has acquired a fluorescent signature. The objective of this study is to develop simple, rapid, commercially viable technique to isolate silk cocoon membrane fluorophores and exploring the possibility of using them as fluorescent dye in bio-imaging. Here, we report an innovative water glass (Na2SiO3) based strategy to isolate the silk cocoon fluorophores. Isolated fluorophore is majorly quercetin derivatives and exhibited remarkable photo- and heat stability. Fluorescence and mass spectrometric analysis confirmed presence of a quercetin derivative. We further used this fluorophore to successfully label the silicate shell of diatom species Nitzschia palea.

  3. 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.

  4. Recent advances in mass spectrometric applications in hydrology

    International Nuclear Information System (INIS)

    The recent advances in mass spectrometric applications in hydrology include 18O of nitrates and sulphates, 37Cl of chlorides for studying origin of groundwater pollution, 3He/4He for geothermal fluids and analysis, 14C, 36Cl and 129I for dating groundwater by Accelerator Mass Spectrometry (AMS)

  5. Preparation and spectrometric identification of amide derivatives with antimalaric

    International Nuclear Information System (INIS)

    The structures of polymeric compounds using spectrometric analysis of infrared, ultraviolet and protonic magnetic resonance and 13C nuclear magnetic resonance are studied. Some structural models are used such as antimalaric-sulfones and pyrimidinic derivatives, and non-polymeric derivatives of active compounds. A comparative analysis on structures less complexes is shown. (M.J.C.). Spectrums 186 p

  6. 工作场所空气中锡的氢化物发生-原子荧光光谱测定法%Determination of Tin in the air by hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    陈峰; 谢超

    2012-01-01

    [Objective] To study the method for determination of tin in workplace air by hydride generation-atomic fluorescence spectrometry. [Methods]The electric hot plate was chosen to digest membrane, with aqua regia as digestive juice. Appropriate instrument conditions were chosen for detection. [Results]The calibration curve was linear in the range of 0-100 μg/L {R =0.999 7). The RSD of standard solution with different concentration was 0.82% -3.87 % , the recoveries were 98.0% -102.7% , and the detection limit was 0.090 μg/ml. [ Conclusion] Hydride generation - atomic fluorescence spectrometry has characteristics of high sensitivity, less interference, selectivity, accuracy, etc. And to do it with aqua regia digestion are appropriate fordetennination of tin in various workplaces.%目的 研究氢化物发生一原子荧光光谱法测定工作场所空气中的锡.方法 电热板消化采样滤膜,选择用王水做消化液消解,选择适宜的仪器工作条件进行检测.结果 在0 ~ 100 μg/L线性范围内,相关系数为0.9997,不同浓度标准溶液的相对标准偏差在0.82%~3.87%之间,加标回收率在98.0%一102.7%之间,方法检出限为0.090 μg/ml.结论 氢化物发生一原子荧光光谱法具有灵敏度高、干扰少、选择性好、准确度高等优点,而用王水做消化液适用于各种作业场所中锡的测定.

  7. 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。

  8. 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.

  9. A single-atom detector integrated on an atom chip: fabrication, characterization and application

    Science.gov (United States)

    Heine, D.; Rohringer, W.; Fischer, D.; Wilzbach, M.; Raub, T.; Loziczky, S.; Liu, XiYuan; Groth, S.; Hessmo, B.; Schmiedmayer, J.

    2010-09-01

    We describe a robust and reliable fluorescence detector for single atoms that is fully integrated on an atom chip. The detector allows spectrally and spatially selective detection of atoms, reaching a single-atom detection efficiency of 66%. It consists of a tapered lensed single-mode fiber for precise delivery of excitation light and a multi-mode fiber to collect the fluorescence. The fibers are mounted in lithographically defined holding structures on the atom chip. Neutral 87Rb atoms propagating freely in a magnetic guide are detected and the noise of their fluorescence emission is analyzed. The variance of the photon distribution allows us to determine the number of detected photons per atom and from there the atom detection efficiency. The second-order intensity correlation function of the fluorescence shows near-perfect photon anti-bunching and signs of damped Rabi oscillations. With simple improvements, one can increase the detection efficiency to 95%.

  10. J Fluorescence

    OpenAIRE

    Resch-Genger, U.; Hoffmann, K.; Nietfeld, W; A. Engel; Neukammer, J.; Nitschke, R.; Ebert, P.; Macdonald, R

    2005-01-01

    The scope of this paper is to illustrate the need for an improved quality assurance in fluorometry. For this purpose, instrumental sources of error and their influences on the reliability and comparability of fluorescence data are highlighted for frequently used photoluminescence techniques ranging from conventional macro- and microfluorometry over fluorescence microscopy and flow cytometry to microarray technology as well as in vivo fluorescence imaging. Particularly, the need for and requir...

  11. Speciation analysis of mercury in sediments using ionic-liquid-based vortex-assisted liquid-liquid microextraction combined with high-performance liquid chromatography and cold vapor atomic fluorescence spectrometry.

    Science.gov (United States)

    Leng, Geng; Chen, Wenjin; Wang, Yong

    2015-08-01

    An improved novel method based on ionic liquid vortex-assisted liquid-liquid microextraction has been developed for the extraction of methylmercury, ethylmercury and inorganic mercury in sediment samples prior to analysis by high-performance liquid chromatography with cold vapor atomic fluorescence spectrometry. In this work, mercury species were firstly complexed with dithizone, and the complexes were extracted into 1-hexyl-3-methylimidazolium hexafluorophosphate. Key factors that affect the extraction efficiency of mercury species, such as type and amount of ionic liquid and chelatants, extraction time, sample pH, salt effect and matrix effect were investigated. Under the optimum conditions, linearity was found in the concentration range from 0.1-70 ng/g. Limits of detection ranged from 0.037-0.061 ng/g. Reproducibility and recoveries were assessed by extracting a series of six independent sediment samples that were spiked with different concentration levels. Finally, the proposed method was successfully applied in analysis of real sediment samples. In this work, ionic liquids vortex-assisted liquid-liquid microextraction was for the first time used for the extraction of mercury species in sediment samples. The proposed method was proved to be much simpler and more rapid, as well as more environmentally friendly and efficient compared with the previous methods. PMID:25998155

  12. 原子荧光光谱法测定水中砷的方法比对试验%Comparative Test of Arsenic Determination in Water by Using Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘清明

    2011-01-01

    Experimental analysis identifies the conditions of atomic fluorescence spectrometry to determine arsenic in water sam- pie, and performs comparative tests of this method under the optiminum conditions, and the current national standards analysis method GB7485 -87. Results indicates that this method is easy to operate, which can greatly improve the detection efficiency and completely replace current complex national standard analysis operation method.%通过试验分析确定了原子荧光光谱法测定水样中砷的检测条件,并在优化试验条件下与现行砷的国家标准分析方法GB 7485-87进行了样品分析比对实验,试验表明,该方法操作简单方便,历时短,可大大提高检测效率,完全可以代替分析操作复杂繁琐的现行国家标准分析方法。

  13. 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。

  14. 原子荧光法测定水中硒时防止铜干扰的方法%Method of Selenium Determination in Water while Interference-Free from Copper with Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    江梅; 陈刚新; 张恺; 念东; 常江

    2015-01-01

    The determination of selenium in water through atomic fluorescence spectrometry method will be interfered by copper. A lot of experiment for increasing concentration of hydrochloric acid or dosing ferric chloride was made in order to find the best determination condition of selenium while interference-free from copper,and the accuracy and precision of datum were analyzed. The results show that the optimum conditions are as follows:concentration of hydrochloric acid is 20% or 0. 6 mL 10 g / L ferric chloride is added. The method is simple and accurate for the determination of selenium in water.%原子荧光法测定水中硒时,铜元素的存在会对硒的测定造成干扰。该文通过大量试验优化条件参数,增加盐酸浓度或加入氯化铁溶液,总结出测定水中硒去除铜干扰的最佳条件,并对该条件下的精密度和准确度进行了评估。结果表明盐酸浓度20%或加入0.6 mL 10 g / L的氯化铁能有效抑制铜元素对硒的干扰,且操作简便、数据准确可靠。

  15. 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。

  16. Determination of Elements in Fish Glue by Microwave Digestion-Atomic Fluorescence Spectrometry%微波消解-原子荧光光谱法测定鱼胶中的元素含量

    Institute of Scientific and Technical Information of China (English)

    丁冶春; 蓝海英; 范小娜; 熊威斌; 程金刚; 张杰

    2012-01-01

    采用微波消解-原子荧光光谱法测定了鱼胶中砷、汞、硒、镉的含量.结果表明,在最佳试验条件下,砷、汞、硒、镉的检出限分别为0.305、0.016、0.082、0.039 ng/mL,样品中4种元素的加标回收率为96.5%~106.2%,可满足鱼胶中的重金属分析.%The content of elements in fish glue, including arsenicum(As), mercury (Hg), selenium(Se) and cadmium(Cd), were determined by microwave digestion-atomic fluorescence spectrometry. The results showed that the detection limits of As, Hg, Se and Cd were 0.305, 0.016, 0.082 and 0.039 ng/mL respectively under the optimized conditions. The recovery was in the range of 96.5%~106.2%, which met the needs of for detecting elements in fish glue.

  17. 微波消解-原子荧光光谱法测定中草药中砷和汞%Determination of Arsenic and Mercury in Chinese Herbal Medicine by Microwave Digestion-Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    朱琳; 曾晓丹; 朱秀影

    2013-01-01

    To determine the contents of arsenic and mercury in Chinese traditional medicine silverweed cinquefoil root,samples were treated by microwave digestion and were determined by atomic fluorescence spectrometry.Under the optimized conditions,the detection limits of As and Hg were 0.235 ng/mL and 0.073 ng/mL,and recovery for As and Hg were 90.74%-4.30% and 94.50%-101.50%,respectively.This method was proved to be fast,simple,convenient,accurate and sensitive.It provides a good alternative for the determination of the poisonous elements in Chinese traditional medicine.%采用微波消解处理样品,利用双通道原子荧光光谱法测定中药材杜仲中As和Hg的含量.最佳实验条件下,As、Hg的检出限分别为0.235、0.0773 ng/mL,回收率在90.74%~94.30%、90.57%~101.50%之间.方法快速、简便、准确且灵敏度高,为中药材中重金属含量测定提供了较好的方法.

  18. 液相色谱-原子荧光联用法测定鱼油中的甲基汞%Determination of methylmercury in fish oil by interface technique coupled high performance liquid chromatography with atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    徐君辉; 周向阳; 沈飚; 秦德元

    2011-01-01

    先后采用10% KOH+ 1%硫脲和20% HCl提取鱼油样品,用液相色谱-原子荧光联用技术测定样品中的甲基汞含量.试验结果表明,线性范围在0~ 10 μg/L之间,相关系数为0.999 3,检出限为0.2 μg/L,加标回收率在96.0%~105.0%之间,相对标准偏差小于5%.该方法快速、简便、准确.%Methylmercury was extracted from fish oil sample with 10% potassium hydroxide and 1% thio-urea, then with 20% hydrochloric acid, and then was determined by interface technique coupled high performance liquid chromatography with atomic fluorescence spectrometry. The results showed that the linear range was between 0 and 10 μg/L,the linear coefficient was 0.999 3 ,the detection limit was 0.2 μg/ L,recovery was between 96.0% and 105. 0% ,the relative standard was less than 5%. The method was rapid, simple, and accurate.

  19. Determination of arsenic releases from glass infusion bottles of drug packaging materials by hydride generation-atomic fluorescence spectrometry%玻璃输液瓶中砷浸出量的原子荧光光谱法测定

    Institute of Scientific and Technical Information of China (English)

    周红娇

    2011-01-01

    目的:建立氢化物发生-原子荧光光谱法HG-AFS测定药包材中玻璃输液瓶的砷浸出量方法.方法:样品液直接用原子荧光光谱法测定,并对HG-AFS工作参数及条件进行优化和选择.结果:标准曲线线性良好,相关系数r=0.999 4,检出限0.064 μg/L,回收率为97.80%,RSD为2.04%.结论:原子荧光光谱法简便、快速准确、灵敏度高.%Objective: To establish a method for determination of arsenic release from Glass Infusion bottles of drug packaging materials by hydride generation-atomic fluorescence spectrometer (HG-AFS). Methods: Sample solutions were directly determined by HG-AFS. Operation parameters of HG-AFS and condition were optimized and selected. Results: A good linearity was obtained (r=0.999 4). The detection limit was 0.064 μg/L. The recovery was 97.80%. RSD was 2.04%.Conclusion: The HG-AFS method is simple and fast with high sensitivity.

  20. 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.

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

    International Nuclear Information System (INIS)

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

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

    Institute of Scientific and Technical Information of China (English)

    沈治荣; 梁聪; 甘丽; 何红莲

    2011-01-01

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

  3. Challenges and recent advances in mass spectrometric imaging of neurotransmitters

    OpenAIRE

    Gemperline, Erin; Chen, Bingming; Li, Lingjun

    2014-01-01

    Mass spectrometric imaging (MSI) is a powerful tool that grants the ability to investigate a broad mass range of molecules, from small molecules to large proteins, by creating detailed distribution maps of selected compounds. To date, MSI has demonstrated its versatility in the study of neurotransmitters and neuropeptides of different classes toward investigation of neurobiological functions and diseases. These studies have provided significant insight in neurobiology over the years and curre...

  4. Electrospray Ionization Mass Spectrometric Analysis of Highly Reactive Glycosyl Halides

    Directory of Open Access Journals (Sweden)

    Lajos Kovács

    2012-07-01

    Full Text Available Highly reactive glycosyl chlorides and bromides have been analysed by a routine mass spectrometric method using electrospray ionization and lithium salt adduct-forming agents in anhydrous acetonitrile solution, providing salient lithiated molecular ions [M+Li]+, [2M+Li]+ etc. The role of other adduct-forming salts has also been evaluated. The lithium salt method is useful for accurate mass determination of these highly sensitive compounds.

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

    Science.gov (United States)

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

    2014-11-01

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

  6. 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.

  7. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    Energy Technology Data Exchange (ETDEWEB)

    1981-01-01

    Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, impurity content. The following analytical procedures, which are described in detail, are designed to show whether or not a given material meets specifications: uranium by ferrous sulfate reduction in phosphoric acid and dichromate titration method; uranium and oxygen uranium atomic ratio by the ignition (gravimetric) impurity correction method; oxygen to uranium atomic ratios by the polarographic method; carbon (total) by direct combustion-thermal conductivity method; total chlorine and fluorine by pyrohydrolysis ion-selective electrode method; moisture by the coulometric, electrolytic moisture analyzer method; nitrogen by the Kjeldahl method; total sulfur by distillation-spectrophotometric method; isotopic uranium composition by multiple-filament surface-ionization mass spectrometric method; spectrochemical determination of trace elements in high-purity uranium dioxide; volatile fluoride impurities by spectrochemical method using the rotating-disk spark technique; spectrochemical determination of silver by gallium oxide carrier D-C arc technique; rare earths by copper spark-spectrochemical method; impurity elements by a spark-source mass spectrographic method; surface area by nitrogen absorption method; total gas in reactor-grade uranium dioxide pellets; thorium and rare earth elements by spectroscopy; hydrogen by inert gas fusion; and uranium isotopic analysis by mass spectrometry. (JMT)

  8. 原子荧光光谱法测定不同产地郁金中砷和硒含量%Determination of Trace Arsenic and Selenium in Curcuma aromatica with Microwave Decomposition-Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    刘艳清; 汪洪武; 蔡璇

    2014-01-01

    After microwave decomposition, the contents of arsenic and selenium in eleven Curcuma aromatica samples were determined by hydride generation atomic fluorescence spectrometry, and plant standard reference materials were used to verify the accuracy and the precision of the analytical method. The experimental conditions were optimized. Under the optimum conditions, there was a good linear relationship between the fluorescence intensity and the contents of arsenic and selenium in the range of 0-20 μg/L with a correlation coefficient of 0.999 8 and 0.999 3, respectively. The recovery rate of arsenic and selenium were in the range of 97.15%-102.87%and 98.35%-101.76%. The results indicated that the contents of arsenic and selenium in different habits of Curcuma aromatica were significant deviation.%应用AFS-930型双道原子荧光光度计,采用湿法消解方式,在选定仪器工作条件下,建立了原子荧光光谱法测定郁金中砷和硒。以工作曲线法测定了不同产地郁金中砷和硒的含量,并用植物标准参考物质评价了分析方法的准确度。在0~20.0μg/L范围内As及Se的线性良好,线性回归方程为:As:If=48.9908 c+55.2433(r=0.9998);Se:If=49.3717 c+46.5837(r=0.9993),砷和硒的回收率分别为97.15%~102.87%和98.35%~101.76%。研究结果表明不同产地郁金中As和Se的含量存在较大差异。

  9. Inductively coupled plasma atomic emission spectrometric determination of silicon, phosphorus, manganese and titanium in ferroaluminum alloy%电感耦合等离子体原子发射光谱法测定铝铁合金中硅磷锰钛

    Institute of Scientific and Technical Information of China (English)

    侯社林; 李存根; 陈延昌; 李建国; 苏彬

    2012-01-01

    Analysis conditions for the determination of silicon, phosphorus, manganese and titanium in ferroaluminum alloy were investigated by inductively coupled plasma atomic emission spectrometry(ICP-AES). Thus a novel determination method was established. After ferroaluminum alloy sample was decomposed by hydrochloric acid, nitric acid and hydrofluoric acid, silicon, phosphorus, manganese and titanium in the test solution were determined by ICP-AES with atomizer and rectangular tubes resistant to hydrofluoric acid under the conditions of radio frequency power of 1 150 W, atomization pressure of 0. 22 MPa, auxiliary gas flow rate of 0. 5 L/min, peristaltic pump speed of 50 r/min, long-wave exposure time of 5 s and shortwave exposure time of 15 s. The overlap interference of spectral lines was eliminated by selecting the spectral line with appropriate sensitivity and exemption from interference as the analytical line of measured element, and the background interference of iron and aluminum were deducted by background correction method. This method has been used for the determination of silicon, phosphorus, manganese, titanium in ferroaluminum alloy sample. It was found that the results were consistent with those obtained by wet method, and the relative standard deviations were not more than 3. 0%.%考察了用电感耦合等离子体原子发射光谱法(ICP-AES)测定铝铁合金中硅、磷、锰和钛的分析条件并建立了测定方法.铝铁合金试样经盐酸、硝酸和氢氟酸分解,在射频功率为1 150 W、雾化压力为0.22 MPa、辅助气流量为0.5 L/min、蠕动泵泵速为50 r/min、长波曝光时间为5 s、短波曝光时间为15s的条件下,使用耐氢氟酸的雾化器和矩管,以ICP-AES测定了试液中硅磷锰钛.通过选择灵敏度适宜和没有干扰的谱线作为被测元素的分析线消除了谱线的重叠干扰,铁铝产生的背景干扰采用背景校正方法扣除.本法已用于铝铁合金样品中硅、磷、锰和

  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.

    Science.gov (United States)

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

    2014-02-01

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

  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 in Drinking Water by Hydride Atomic Fluorescence Spectrometry%评定氢化物原子荧光法测定生活饮用水中砷的测量不确定度分析

    Institute of Scientific and Technical Information of China (English)

    应绍先; 泽周艳

    2015-01-01

    目的建立氢化物原子荧光法测定生活饮用水中砷的不确定度评定方法,给出不确定度,为提高检测质量提供依据,评定测定结果,找出主要影响因素。方法根据有关生活饮水检验的科学方法和法律法规规定的有关生活饮用水的金属指标GB/T5750,6-2006,应用测量不确定度理论,建立检测方法的数学模型,通过对标准系列稀释过程以及水样的量取等相关过程的讨论分析,讨论每个过程的不确定度分量,并对影响不确定度的因素进行评估。结果对扩展不确定度影响比较大的两大因素分别是标准系列稀释过程和仪器测量精密度过程。讨论与体积相关的四个分项的不确定度,并将标准系列稀释过程作为讨论的重点。结论此方法适用于评估氢化物原子荧光法测定生活饮用水中砷含量的不确定度。%Objective To build the method of evaluation of determination of arsenic in drinking water by Hydride Generation Atomic Fluorescence Spectrometry with uncertainty,give the uncertainty, provide a basis for improving the detection quality, determination of evaluation results,and find out the main influencing factors.Methods The mathematical model established detection method was built used the theory of measurement uncertainty according to the metal indicators related to drinking water drinking water GB/T5750,6-2006 provisions on inspection of scientific methods and laws and regulations,the standard serial dilution process and the amount of water and other related processes was discussed and analysised,uncertainty component of each process was discussed and ef ect of uncertain factors were valuated.Results Two major factors with greater impact on expanded uncertainty were the standard serial dilution process and instrument measurement precision process.The four sub volume and related uncertainty were discuss,and the focus of discussion was the standard serial dilution process.Conclusion This

  13. 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

    International Nuclear Information System (INIS)

    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)

  14. 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。

  15. 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.

  16. Determination of Mercury in Peanut by Microwave Digestion Atomic Fluorescence Spectrometry%微波消解原子荧光光度法测定花生样品中的汞

    Institute of Scientific and Technical Information of China (English)

    何超君; 张激光; 卢思桥

    2012-01-01

    Trace Hg in peanut was determined by atomic fluorescence spectrometry(AFS) with microwave digestion. The detection limit of mercury was 0.000 4 μg/g(n=11), the linear range for mercury was 0.001~6 μg/g, the correlation coefficieni was 0.999 95,and relative standard deviation (RSD,n=7) was in the range of 4.84%~S 30%, the recovery of the method was in the range of 91.00%~114.00%, The experiment results show that the concentration of Hg is lower than the maximum allowable level of Hg in our food standard.The proposed method is rapid and convenient, the result is accurate and reliable, and it is suitable for the determination of trace Hg in peanut.%采用微波消解技术—原子荧光光度法测定花生样品中痕量Hg.方法检出限为0.0004μg/g,线性范围:0.0001~6 μg/g,相关系数r=0.999 95,相对标准偏差(RSD,n=7)4.84%~5.30%,加标回收率在91%~114%之间.实验证明:花生中有害元素Hg的含量远低于我国粮食(成品粮)总Hg允许限标准.方法简便、快速,结果准确、可靠,能够满足花生样品中痕量Hg的测定.

  17. 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).

  18. 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)

  19. 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

  20. 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.

  1. Monoclonal antibody-based time-resolved fluorescence immunoassays for daidzein, genistein and equol in blood and urine

    DEFF Research Database (Denmark)

    Talbot, Duncan C.S.; Ogborne, Richard M.; Dadd, Tony;

    2007-01-01

    Background: Time-resolved fluorescence immunoessays (TR-FIAs) for phytoestrogens in biological samples are an alternative to mass spectrometric methods. These immunoessays were used to test urne and plasma samples from individuals in a dietary trial aimed at determining the efficacy of dietary is...

  2. 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 ...

  3. Fluorescent refrigeration

    Science.gov (United States)

    Epstein, Richard I.; Edwards, Bradley C.; Buchwald, Melvin I.; Gosnell, Timothy R.

    1995-01-01

    Fluorescent refrigeration is based on selective radiative pumping, using substantially monochromatic radiation, of quantum excitations which are then endothermically redistributed to higher energies. Ultimately, the populated energy levels radiatively deexcite emitting, on the average, more radiant energy than was initially absorbed. The material utilized to accomplish the cooling must have dimensions such that the exciting radiation is strongly absorbed, but the fluorescence may exit the material through a significantly smaller optical pathlength. Optical fibers and mirrored glasses and crystals provide this requirement.

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

    Institute of Scientific and Technical Information of China (English)

    高向阳; 王银娟; 卢彬

    2011-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

    刘金; 彭元; 陈红梅; 程先忠

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Thierig, D.

    1982-01-01

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

  8. The hydrolysis of aluminium, a mass spectrometric study

    OpenAIRE

    Sarpola, A.

    2007-01-01

    Abstract This thesis is focused on the hydrolysis of aluminium, the polymerisation of the hydrolysis products, and how these can be monitored by mass spectrometric methods. The main aim of this research is to figure out how the aqueous speciation of aluminium changes as a function of pH (3.2–10), concentration (1–100 mM), reaction time (1s–14d), and counter anion (Cl-, SO42-, HCOO-). The method used was electrospray mass spectrometry. The results showed more variable speciation than those ...

  9. Visualization of High Resolution Spatial Mass Spectrometric Data during Acquisition

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, Mathew; Heath, Brandi S.; Laskin, Julia; Li, Dongsheng; Liu, Ellen C.; Hui, Katrina L.; Kuprat, Andrew P.; Kleese van Dam, Kerstin; Carson, James P.

    2012-08-28

    Mass Spectrometric Imaging (IMS) allows the generation of 2D ion density maps that help visualize molecules present in sections of tissues and cells. The combination of spatial and mass resolution results in large and complex data sets that require powerful and efficient analysis and interpretation. In this paper, a graphical user interface (GUI) that can visualize the large data during data acquisition itself is presented. The program also has the ability to perform processing and analysis of the dataset. The various functions of the GUI including visualization of mass spectra, generation of 2D maps for selected species, manipulation of the heat maps, and peak identification are also presented.

  10. Mass spectrometric imaging of ginsenosides localization in Panax ginseng root

    OpenAIRE

    Taira, Shu; Ikeda, Ryuzo; Yokota, Naohiko; OSAKA, Issey; Sakamoto, Manabu; Kato, Mitsuro; Sahashi, Yuko

    2010-01-01

    We succeeded in performing mass spectrometric imaging (MSI) of the localization of ginsenosides (Rb_1, Rb_2 or R_c, and Rf) in cross-sections of the Panax ginseng root at a resolution of 100 μm using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Tandem mass spectrometry (MS/MS) of alkali metal-adducted ginsenoside ions revealed structural information of the corresponding saccharides and agricones. MALDI-MSI confirmed that localization of ginsenosides in the cortex ...

  11. Identification and expression of a gfpK79R mutant of green fluorescent protein

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A mutant strain of E.coli showing strong green fluorescence is obtained during the study of cloning and expression of blue fluorescent protein gene bfp. A recombinant plasmid pHN122 has been isolated. It is demonstrated by enzyme digestion, subcloning and sequence analysis that it contains both of bfp and gfpK79R mutant genes. The results of spectrometric analysis show that GFPK79R expressed by pHN122 is the same as the wild type GFP, but its fluorescent intensity is increased 1.25~2.44-fold.

  12. 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.

  13. 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

  14. 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

  15. 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.

  16. 微波消解氢化物原子荧光法测定食品中的砷和汞%Simultaneous determination of arsenic and mercury in food by microwave digestion and atomic fluorescence spectroscopy

    Institute of Scientific and Technical Information of China (English)

    郭同兵; 黄谦; 刘剑波

    2011-01-01

    A process of closed and high pressure microwave digestion with atomic fluorescence spectrometer for simultaneously determine As and Hg in food was established. Compared with traditional wet digestion method, the microwave digestion features simple operation, fast, little interference and excellent process controllability. After detect rice, meat, mineral water.aquatic product and so on, we find the detection limits for arsenic and mercury were 0. 030 6 μg/L and 0. 005 2 μg/L respectively. The relative standard deviation for As was 2. 40%,while 1. 39% for Hg. The recovery for As was in the rang of 99. 4% - 101. 2% and 94. 5%~ 106. 5% for Hg. And the As correlation coefficient was 0. 999 7, while the Hg was 0. 999 6. The result is fine, and is fit for simultaneously determine As and Hg in food.%采用高压密闭微波消解氢化物原子荧光法对食品中砷、汞进行同时测定,并与传统的湿法消解进行比较.结果表明:该法具有操作简单、快速、干扰少、良好的过程可控性等优点.通过对大米、肉类罐头、矿采水和水产品等样品的检测,发现砷、汞的检出限分别为0.0306,0.0052 μg/L;相对标准偏差(RSD):砷为2.40%,Hg为1.39%;回收率:As为99.4%~101.2%,Hg为94.5%~106.5%;相关系数(r):As为0.999 7,Hg为0.999 6.结果良好,适用于多种食品中砷和采的同时检测.

  17. 断续流动原子荧光法测定铅锡合金中的痕量锑%Determination of Trace Amount of Antimony in Lead-tin Alloy by Intermittent Flow Atomic Fluorescence Spectrometry

    Institute of Scientific and Technical Information of China (English)

    马毅红; 尹艺青; 陈玉珍

    2012-01-01

    目的:建立氢化物发生双道原子荧光法测定铅锡合金中锑含量的方法,为测定铅锡合金中锑提供依据。方法:选择了最佳的仪器条件,进行样品处理方法、KBH4浓度、检出限、回收率等研究。结果:本方法的标准曲线方程y=157.56x-2.3962,相关系数γ=0.9999,线性范围为0~40μg/L,精密度为1.3%,检出限为0.0304μg/L,回收率达115%。结论:本方法操作简单、快速、灵敏度高、干扰少,可获得满意的结果。%Purpose: A analytical method is recommended for determination of Trace Amount of Antimony in Lead-Tin Alloy by hydride generation double channel atomic fluorescence spectrometry,which provides basis for its measurement.Methods: Optimum condition for the instrument determination is applied to conduct researches relating to the method of sampling,concentration of KBH4,detection limits and recovery rate.Results: The standard curve of the linear equation was y=157.56x-2.3962 with correlation coefficient γ = 0.9999 and linear range of 0~40 μg/L.The precision and the detection limits were 1.3 % and 0.0304 μg/L respectively while the returns-ratio achieves 115 %.Conclusion: The method is easy,fast,highly sensitive and with no much interference during the operation,which can lead to satisfactory results.

  18. 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。

  19. Mass spectrometric detection of radiocarbon for dating applications

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-01-15

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

  20. Mass spectrometric detection of radiocarbon for dating applications

    Science.gov (United States)

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

    2013-01-01

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

  1. Atom Chips

    CERN Document Server

    Folman, R; Cassettari, D; Hessmo, B; Maier, T; Schmiedmayer, J; Folman, Ron; Krüger, Peter; Cassettari, Donatella; Hessmo, Björn; Maier, Thomas

    1999-01-01

    Atoms can be trapped and guided using nano-fabricated wires on surfaces, achieving the scales required by quantum information proposals. These Atom Chips form the basis for robust and widespread applications of cold atoms ranging from atom optics to fundamental questions in mesoscopic physics, and possibly quantum information systems.

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

    International Nuclear Information System (INIS)

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

  3. Flame atomic absorption spectrometric determinations of some trace metals after coprecipitation with gold-APDC

    International Nuclear Information System (INIS)

    Complete text of publication follows. For the determination of trace metals in various samples, preconcentration is an inevitable step to overcome interferences. Among various techniques for the separation of trace metals proposed until now, coprecipitation is one of the most useful ones. Many different coprecipitation procedures including use of organic and inorganic collectors have been developed. So far, in the literature, it is reported that APDC, NaDDTC, PAN, TAR, Oxine, etc. as chelating agent for metal-chelate collector have been extensively used for coprecipitation of trace metals. However, metal chelates, especially dithocarbamates, as collectors are ideal for their sensitivities, simplicities and tolerances to interferences.Therefore, in the present work, fundamental studies on the coprecipitation with gold/APDC chelate have been carried out for determination of trace metals in environmental samples by FAAS with microinjection. According to our literature survey, gold/APDC is not used for the coprecipitation of heavy metal ions, until now. In this work, the coprecipitation was carried out in a centrifuge tube. Firstly, the main factors, such as amount of coprecipitant reagent and carrier element, pH of the solution, standing time, sample volume and diverse ions, affecting the coprecipitation of some trace metals were evaluated. Under optimized conditions, the recoveries of Cu, Ni, Pb and Cd were ≥ 95 %. R.S.D. values for ten replicates were lower than 5.0 %. Preconcentration factors were found to be 20. The coprecipitation was applied to various water samples and non-alcoholic beverage.

  4. 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.

  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 profiling of flavonoid glycoconjugates possessing isomeric aglycones.

    Science.gov (United States)

    Abrankó, László; Szilvássy, Blanka

    2015-01-01

    In fields such as food and nutrition science or plant physiology, interest in untargeted profiling of flavonoids continues to expand. The group of flavonoids encompasses several thousands of chemically distinguishable compounds, among which are a number of isobaric compounds with the same elemental composition. Thus, the mass spectrometric identification of these compounds is challenging, especially when reference standards are not available to support their identification. Many different types of isomers of flavonoid glycoconjugates are known, i.e. compounds that differ in their glycosylation position, glycan sequence or type of interglycosidic linkage. This work focuses on the mass spectrometric identification of flavonoid glycoconjugate isomers possessing the same glycan mass and differing only in their aglycone core. A non-targeted HPLC-ESI-MS/MS profiling method using a triple quadrupole MS is presented herein, which utilizes in-source fragmentation and a pseudo-MS(3) approach for the selective analysis of flavonoid glycoconjugates with isomeric/isobaric aglycones. A selective MRM-based identification of the in-source formed isobaric aglycone fragments was established. Additionally, utilizing the precursor scanning capability of the employed triple quadrupole instrument, the developed method enabled the determination of the molecular weight of the studied intact flavonoid glycoconjugate. The versatility of the method was proven with various types of flavonoid aglycones, i.e. anthocyanins, flavonols, flavones, flavanones and isoflavones, along with their representative glycoconjugates. The developed method was also successfully applied to a commercially available sour cherry sample, in which 16 different glycoconjugates of pelargonidin, genistein, cyanidin, kaempferol and quercetin could be tentatively identified, including a number of compounds containing isomeric/isobaric aglycones. PMID:25601677

  8. 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

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

    Science.gov (United States)

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

    2006-12-15

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

  10. Determination of arsenic in titanium dioxide by hydride generation atomic fluorescence spectrometry%氢化物发生-原子荧光光谱法测定二氧化钛中砷

    Institute of Scientific and Technical Information of China (English)

    王勇; 王维; 刘元清; 刘林; 龚厚亮

    2016-01-01

    For the detection of arsenic in titanium dioxide ,the sample was usually dissolved with nitric acid‐hydrochloric acid‐hydrofluoric acid system .However ,this pretreatment method had the following prob‐lems :the titanium was easily hydrolyzed;the digestion time was relatively long .In the experiment ,the dissolution method of titanium dioxide sample with sulfuric acid‐ammonium sulfate system was proposed . The problems above were solved .Moreover ,the reaction was mild .Accordingly ,the determination meth‐od of arsenic in titanium dioxide by hydride generation atomic fluorescence spectroscopy (HG‐AFS) was established .The results showed that the mass concentration of arsenic in range of 0.50‐20 μg/L had good linear relationship with the corresponding absorbance .The linear correlation coefficient was 0.999 8 .The detection limit of method was 0.05 μg/L .The interference test results indicated that the coexisting ele‐ments in matrix titanium sample did not interfere with the determination .The proposed method was ap‐plied to the analysis of actual sample ,and the found results were consistent with those obtained by induc‐tively coupled plasma mass spectrometry (ICP‐MS) .The relative standard deviation (RSD ,n=11) was less than 5% .The recoveries of standard addition were between 95% and 101% .%二氧化钛中砷的检测方法中,样品前处理多数采用硝酸‐盐酸‐氢氟酸混酸体系溶解,而采用此法处理样品,会存在钛容易水解且消解时间较长的问题。实验提出了硫酸‐硫酸铵体系溶解二氧化钛样品的方法,不仅解决了上述问题且反应温和,并据此建立了氢化物发生‐原子荧光光谱法(HG‐AFS)测定二氧化钛样品中砷的方法。实验表明,砷的质量浓度在0.50~20μg/L范围内与其对应的吸光度呈线性关系,线性相关系数为0.9998,方法检出限为0.05μg/L。干扰试验表明,基体钛样品中的共存元素均不

  11. 氢化物发生原子荧光法测定稻田土中的锑形态%Determination of antimony species in rice paddy soils by hydride generation atomic fluorescence spetrometry

    Institute of Scientific and Technical Information of China (English)

    郎春燕; 周英; 赖晨焕

    2012-01-01

    Antimony species in rice paddy soils in east suburb of Chengdu were determined by hydride generation-atomic fluorescence spectrometry using aqua regia as a digestant and sequential extraction method. The detection limit of Sb was 0. 108 μg/L,and the recoveries of Sb were 96. 9% ~ 104. 8%. The results showed that the interferences from Cu2+ 、Co2+ 、Se4+ 、Sn2 +、Zn2+、Pb2+、As3+ 、As5+ 、Hg2+ which possibly existed in soils could be efficiently eliminated by using the mixture of thiourea and ascorbic acid. The concentrations of antimony were in the range from 0. 92 mg/kg to 2. 52 mg/kg in samples. The average concentration was 1. 76 mg/kg. The results were not much higher than the standard concentrations of Sb in soils in SiChuan( ≈1. 70 mg/kg, 1991). In the horizontal direction, the distribution of antimony species was different due to different soil conditions of rice paddy. The concentration of antimony species in the studied rice paddy soils generally followed the direction of residual phase > organic/sulphidic phase > Fe/Mn hydrous oxides > carbonate fraction > cation exchangeable. There was a very small proportion of cation exchangeable which could be easily absorbed by plants. In the vertical direction, the concentrations of antimony species had a decreasing tendency with the increased depth of soil.%采用王水消解及逐级浸提技术,以氢化物发生-原子荧光法对成都东郊稻田土中的Sb形态进行了分析,方法检出限为0.108 μg/L,回收率为96.9%~104.8%.加入硫脲-抗坏血酸溶液后,土壤样品中可能存在的金属离子Cu2+、Co2+、Se4、Sn2+、Zn2+、pb2+、As3+、As5+、Hg2+对Sb的干扰可以有效地消除;样品Sb含量在0.92 ~2.52 mg/kg之间波动,平均值为1.76 mg/kg,与四川省土壤Sb背景浓度(≈1.70 mg/kg,1991)相比相差不大.水平方向上,各形态Sb的浓度因所处稻田条件的不同而分布各异,大体呈以下规律:残渣态>有机/硫化物结合态>铁/锰

  12. 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.

  13. 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

  14. Characterization of used lubricating oil by spectrometric techniques

    International Nuclear Information System (INIS)

    Full text: The engine lubricating oil drags all kinds of impurities generated by wear of internal components. Thus, it is necessary to monitor the physical and chemical properties and concentration of metals in lubricants used to determine the appropriate time to replace them. Moreover, one can monitor the wear of the engines through the levels of metals in oils. To achieve these goals, some detection techniques such as Flame atomic absorption spectrometry (FAAS), Inductively coupled plasma optical emission spectrometry (ICP-OES) and X-ray fluorescence (XRF), have been widely used to determine metals in lubricating oils and also in other oil derivatives. Thus, some of these techniques were used in this study. Also the technique used was Gas chromatography mass spectrometry (GC / MS) for characterization of chromatographic profile of the engine lubricating oil after use. Through the technique of ICP-OES for method of United States Environmental Protection Agency (USEPA) METHOD 6010B - Inductively coupled plasma optical emission spectrometry was performed to characterize metals in lubricating oil motor, using equipment from ICP-OES Perkin-ElmerR OPTIMA 3000 ICP-Winlab and software, obtaining the following identification of metals: barium (Ba), calcium (Ca), lead (Pb), copper (Cu), Chromium (Cr), iron (Fe), magnesium (Mg), molybdenum (Mo) and zinc (Zn). Using the XRF technique, through the equipment EDFRX ShimadzuR model 800HS EDX, Rh tube, applied voltage of 50kV, amperage 100μA, detector Si (Li) cooled with liquid nitrogen and collimator 10mm, we analyzed all the components comprised in the range of Ti to U and Na to SC, identified the following metals: calcium (Ca), zinc (Zn), iron (Fe), copper (Cu), molybdenum (Mo) and nickel (Ni). The characterization was performed by chromatographic methods: USEPA METHOD 5021A - Volatile organic compounds in various sample matrices using equilibrium headspace analysis, USEPA METHOD 8015B - Nonhalogenated Organics Using GC

  15. Atomic Physics

    CERN Document Server

    Foot, Christopher J

    2007-01-01

    This text will thoroughly update the existing literature on atomic physics. Intended to accompany an advanced undergraduate course in atomic physics, the book will lead the students up to the latest advances and the applications to Bose-Einstein Condensation of atoms, matter-wave inter-ferometry and quantum computing with trapped ions. The elementary atomic physics covered in the early chapters should be accessible to undergraduates when they are first introduced to the subject. To complement. the usual quantum mechanical treatment of atomic structure the book strongly emphasizes the experimen

  16. Method of double tracer addition for determining uranium in geological samples by mass spectrometric isotope dilution

    International Nuclear Information System (INIS)

    The present work shows the experimental details on the uranium determination in materials by mass spectrometric isotope dilution technique with double tracer (233U + 235U). The mass discrimination phenomenon effect is studied. The uranium concentration values obtained by mass spectrometric isotope dilution technique with double tracer are compared with other techniques. The influence of the sampling in the accurate determination of uranium in the rock sample is discussed. (author)

  17. 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.

  18. 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.

  19. Atom interferometry

    International Nuclear Information System (INIS)

    We will first present a development of the fundamental principles of atom interferometers. Next we will discuss a few of the various methods now available to split and recombine atomic De Broglie waves, with special emphasis on atom interferometers based on optical pulses. We will also be particularly concerned with high precision interferometers with long measurement times such those made with atomic fountains. The application of atom interferometry to the measurement of the acceleration due to gravity will be detailed. We will also develop the atom interferometry based on adiabatic transfer and we will apply it to the measurement of the photon recoil in the case of the Doppler shift of an atomic resonance caused by the momentum recoil from an absorbed photon. Finally the outlook of future developments will be given. (A.C.)

  20. 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. ᅟ PMID:23690250

  1. 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 .

  2. Atomic physics

    International Nuclear Information System (INIS)

    Research activities in atomic physics at Lawrence Berkeley Laboratory during 1976 are described. Topics covered include: experiments on stored ions; test for parity violation in neutral weak currents; energy conservation and astrophysics; atomic absorption spectroscopy, atomic and molecular detectors; theoretical studies of quantum electrodynamics and high-z ions; atomic beam magnetic resonance; radiative decay from the 23Po,2 levels of helium-like argon; quenching of the metastable 2S/sub 1/2/ state of hydrogen-like argon in an external electric field; and lifetime of the 23Po level of helium-like krypton

  3. 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.

  4. Spectrometric measurements of radioisotope activity in the thyroid

    Science.gov (United States)

    Osko, Jakub; Golnik, Natalia

    2008-01-01

    The results of measurements of iodine 131I and technetium 99mTc uptake in human thyroid, performed with scintillation or semiconductor detectors can exhibit a considerable uncertainty due to the differences in the thyroid position in the patient's neck. Basic physical laws of radiation attenuation and scattering show that the final shape of the registered spectrum should depends on the thyroid position in the neck and on the thickness of the tissue between the thyroid and the detector. The use of the spectrometric measuring method is proposed in this work for determination of the iodine gathering effective depth. The performed studies showed that the measurements results can be used for improving the accuracy of the iodine 131I activity in thyroid measurements and for selection of the group of patients for whom the anatomical position of the thyroid or the spatial distribution of the iodine gathering is much different than the standard one, assumed during the calibration of the counters. The results of the measurements were in agreement with Monte-Carlo calculations of the detector response. The method was used in routine monitoring of occupationally exposed persons, using the thyroid counter. A group of six persons with measurable internal contamination was selected and the measurements were performed on consecutive days, so the results could be registered at decreasing iodine activities in the thyroid. Larger series of measurements were performed at Brodno Regional Hospital in Warsaw, for a group of 95 patients after diagnostic administration of iodine 131I.

  5. Mass spectrometric study of the amipurimycin hexopyranosidic sugar moiety

    Science.gov (United States)

    Almoster Ferreira, M. A.; Borges, C.; Oliveira, M. C.; Pocsfalvi, G.; Rauter, A. P.; Fernandes, A. C.

    1997-11-01

    Amipurimycin is a natural nucleoside that displays a remarkable activity in vitro and in vivo against Pyricularia oryzae, which is responsible for the rice blast disease. Six important precursors for the synthesis of the Amipurimycin sugar moiety were prepared. In order to obtain structural information a mass spectrometric study of these compounds was performed using liquid secondary ion mass spectrometry (LSIMS) with high-energy collision-induced dissociation (CID) experiments on a four-sector instrument. Elimination of methanol is the preferential fragmentation path for five of the six protonated molecules, indicating that protonation plays an important role in the process, whilst for the other protonated molecule loss of water is the main fragmentation. Examination of the [M + Li]+ precursor ion spectra shows that loss of methanol does not occur in three of them, but in the other three gives rise to fairly abundant ions, indicating that in this case methanol elimination implies intramolecular hydrogen transfer, the resulting ion having a very stable structure.

  6. Status of mass spectrometric radiocarbon detection at ETHZ

    Science.gov (United States)

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

    2015-10-01

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

  7. Surface acoustic wave nebulization facilitating lipid mass spectrometric analysis.

    Science.gov (United States)

    Yoon, Sung Hwan; Huang, Yue; Edgar, J Scott; Ting, Ying S; Heron, Scott R; Kao, Yuchieh; Li, Yanyan; Masselon, Christophe D; Ernst, Robert K; Goodlett, David R

    2012-08-01

    Surface acoustic wave nebulization (SAWN) is a novel method to transfer nonvolatile analytes directly from the aqueous phase to the gas phase for mass spectrometric analysis. The lower ion energetics of SAWN and its planar nature make it appealing for analytically challenging lipid samples. This challenge is a result of their amphipathic nature, labile nature, and tendency to form aggregates, which readily precipitate clogging capillaries used for electrospray ionization (ESI). Here, we report the use of SAWN to characterize the complex glycolipid, lipid A, which serves as the membrane anchor component of lipopolysaccharide (LPS) and has a pronounced tendency to clog nano-ESI capillaries. We also show that unlike ESI SAWN is capable of ionizing labile phospholipids without fragmentation. Lastly, we compare the ease of use of SAWN to the more conventional infusion-based ESI methods and demonstrate the ability to generate higher order tandem mass spectral data of lipid A for automated structure assignment using our previously reported hierarchical tandem mass spectrometry (HiTMS) algorithm. The ease of generating SAWN-MS(n) data combined with HiTMS interpretation offers the potential for high throughput lipid A structure analysis. PMID:22742654

  8. Functional proteomics with new mass spectrometric and bioinformatics tools

    International Nuclear Information System (INIS)

    A comprehensive range of mass spectrometric tools is required to investigate todays life science applications and a strong focus is on addressing the needs of functional proteomics. Application examples are given showing the streamlined process of protein identification from low femtomole amounts of digests. Sample preparation is achieved with a convertible robot for automated 2D gel picking, and MALDI target dispensing. MALDI-TOF or ESI-MS subsequent to enzymatic digestion. A choice of mass spectrometers including Q-q-TOF with multipass capability, MALDI-MS/MS with unsegmented PSD, Ion Trap and FT-MS are discussed for their respective strengths and applications. Bioinformatics software that allows both database work and novel peptide mass spectra interpretation is reviewed. The automated database searching uses either entire digest LC-MSn ESI Ion Trap data or MALDI MS and MS/MS spectra. It is shown how post translational modifications are interactively uncovered and de-novo sequencing of peptides is facilitated

  9. 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.

  10. Fluorescence detection: SPIE volume 743

    Energy Technology Data Exchange (ETDEWEB)

    Menzel, E.R.

    1987-01-01

    This book contains proceedings arranged into four sessions. They are: Fluorescence spectroscopic techniques; Fluorescence in analysis and materials characterization; Fluorescence in medicine and biochemistry; and Fluorescence in criminalistics.

  11. 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.

  12. Determination of rare-earth elements in rocks by isotope-excited X-ray fluorescence spectrometry

    DEFF Research Database (Denmark)

    Kunzendorf, Helmar; Wollenberg, H.A.

    1970-01-01

    Isotope-excited X-ray fluorescence spectrometry furnishes a rapid determination of rare-earth elements in unprepared rock samples. The samples are excited by 241Am γ-rays, generating X-ray spectra on a multichannel pulse-height analyser. Gaussian peaks of the Kα and Kβ X-ray energies are treated......-ray spectrometric scan of a longitudinally sliced drill core showed a close correlation between rare-earth abundances and appropriate minerals....

  13. Single hair cocaine consumption monitoring by mass spectrometric imaging.

    Science.gov (United States)

    Porta, Tiffany; Grivet, Chantal; Kraemer, Thomas; Varesio, Emmanuel; Hopfgartner, Gérard

    2011-06-01

    Matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI-MSI) was used to image the distribution of cocaine and its metabolites in intact single hair samples from chronic users down to a concentration of 5 ng/mg. Acquisitions were performed in rastering mode, at a speed of 1 mm/s and in the selected reaction monitoring (SRM) mode on a MALDI triple quadrupole linear ion trap fitted with a high repetition rate laser (1 kHz). Compared to traditional methods based on LC-MS/MS or GC-MS(/MS) which require to segment the hair to obtain spatial resolution, MALDI-MSI, with a straightforward sample preparation beforehand, allowed obtaining a spatial resolution of 1 mm and thus the chronological information about cocaine consumption contained in a single intact hair over several months could be monitored. The analysis time of an intact single hair sample of 6 cm is approximately of 6 min. Cocaine and its metabolites benzoylecgonine, ethylcocaine, and norcocaine were investigated in nine sets of hair samples for forensic purposes. The analyses were accomplished by spraying α-cyano-4-hydroxycinnamic acid (CHCA), 4-chloro-α-cyano-cinnamic acid (Cl-CCA), or (E)-2-cyano-3-(naphthalen-2-yl)acrylic acid (NpCCA) as MALDI matrices. We also propose a rapid strategy for sensitive confirmatory analyses with both MS/MS and MS(3) experiments performed directly on intact hair samples. Since only part of the hair strand is analyzed, additional analyses are possible at any time on the remaining hair from the strand. PMID:21510611

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

    Science.gov (United States)

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

    2009-10-01

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

  15. 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.

  16. Hydrogen--deuterium exchange in water vapor: the mass spectrometric sensitivities and the equilibrium constant

    Energy Technology Data Exchange (ETDEWEB)

    Pyper, J.W.; Dupzyk, R.J.; Friesen, R.D.; Bernasek, S.L.; May, C.A.; Echeverria, A.W.; Tolman, L.F.

    1976-04-21

    The equilibrium constant, K/sub HDO/, for the reaction H/sub 2/O + D/sub 2/O = 2HDO can be expressed as an intensity ratio, I, measured mass spectrometrically, times a sensitivity ratio, S, measured in mass spectrometric calibration experiments. The latter is difficult to measure and previously was assumed to be unity. The 2.4 percent discrepancy between K's from theoretical calculations and direct mass spectrometric measurements might be explained by another value of S. An indirect measurement of S using a pulsed-molecular beam quadrupole mass filter that has a unique three-chamber, three-leak gas inlet system is reported. The results show the sensitivities are probably equal and therefore S = 1. Systematic errors were found in the procedure, however, which precluded an unambiguous test of the theory.

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

    International Nuclear Information System (INIS)

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

  18. Modular mass spectrometric tool for analysis of composition and phosphorylation of protein complexes.

    Directory of Open Access Journals (Sweden)

    Justin D Blethrow

    Full Text Available The combination of high accuracy, sensitivity and speed of single and multiple-stage mass spectrometric analyses enables the collection of comprehensive sets of data containing detailed information about complex biological samples. To achieve these properties, we combined two high-performance matrix-assisted laser desorption ionization mass analyzers in one modular mass spectrometric tool, and applied this tool for dissecting the composition and post-translational modifications of protein complexes. As an example of this approach, we here present studies of the Saccharomyces cerevisiae anaphase-promoting complexes (APC and elucidation of phosphorylation sites on its components. In general, the modular concept we describe could be useful for assembling mass spectrometers operating with both matrix-assisted laser desorption ionization (MALDI and electrospray ionization (ESI ion sources into powerful mass spectrometric tools for the comprehensive analysis of complex biological samples.

  19. 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.

  20. 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.

  1. Determination of Arsenic in Southern Jiangxi Navel Orange Pulp and Peel by Wet Digestion—Atomic Fluorescence Spectrometry%湿法消解-原子荧光光谱法测定赣南脐橙果皮和果肉中的砷含量

    Institute of Scientific and Technical Information of China (English)

    徐媛; 姚明印; 刘木华; 雷泽剑

    2012-01-01

    With a view to detect the heavy metal element in fruits, the contents of element arsenic in peel and the fruit pulp of Southern Jiangxi navel orange were determined by wet digestion-atomic fluorescence spec-trometry. The fruit pulp and peel were preconditioned by wet digestion and then detected by atomic fluorescence spectrometry. The results showed that trace arsenic was contained in pulp and peel, the average amount of arsenic per kg of Southern Jiangxi navel orange was 0.096 mg(peel) ,0.020 (pulp) respectively, the total arsenic content in Southern Jiangxi navel orange conforms to China' s safety and health indicators. The element arsenic in Southern Jiangxi navel orange mainly rests in the peel.%以检测水果中有害元素(以As为例)含量为目的,实验选用赣南脐橙作为样品,采用湿法消解-原子荧光光谱法测定其果皮和果肉中有害元素砷的含量.实验先用湿法消解的方法预处理赣南脐橙的果皮和果肉,制备好样品,再用原子荧光光谱仪测定样品中痕量砷的含量.结果表明,脐橙果皮和果肉中含有微量砷元素,所检测的脐橙中平均含砷量为0.096 mg/kg(果皮)、0.020 mg/kg(果肉),脐橙样品中元素砷主要累积在果皮.

  2. Prospects in Analytical Atomic Spectrometry

    CERN Document Server

    Bolshakov, A A; Nemets, V M

    2006-01-01

    Tendencies in five main branches of atomic spectrometry (absorption, emission, mass, fluorescence and ionization spectrometry) are considered. The first three techniques are the most widespread and universal, with the best sensitivity attributed to atomic mass spectrometry. In the direct elemental analysis of solid samples, the leading roles are now conquered by laser-induced breakdown and laser ablation mass spectrometry, and the related techniques with transfer of the laser ablation products into inductively-coupled plasma. Advances in design of diode lasers and optical parametric oscillators promote developments in fluorescence and ionization spectrometry and also in absorption techniques where uses of optical cavities for increased effective absorption pathlength are expected to expand. Prospects for analytical instrumentation are seen in higher productivity, portability, miniaturization, incorporation of advanced software, automated sample preparation and transition to the multifunctional modular archite...

  3. 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.

  4. 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%.

  5. Atomic secrecy

    International Nuclear Information System (INIS)

    An article, The H-Bomb Secret: How We Got It, Why We're Telling It, by Howard Morland was to be published in The Progressive magazine in February, 1979. The government, after learning of the author's and the editors' intention to publish the article and failing to persuade them to voluntarily delete about 20% of the text and all of the diagrams showing how an H-bomb works, requested a court injunction against publication. Acting under the Atomic Energy Act of 1954, US District Court Judge Robert W. Warren granted the government's request on March 26. Events dealing with the case are discussed in this publication. Section 1, Progressive Hydrogen Bomb Case, is discussed under the following: Court Order Blocking Magazine Report; Origins of the Howard Morland Article; Author's Motives, Defense of Publication; and Government Arguments Against Disclosure. Section 2, Access to Atomic Data Since 1939, contains information on need for secrecy during World War II; 1946 Atomic Energy Act and its effects; Soviet A-Bomb and the US H-Bomb; and consequences of 1954 Atomic Energy Act. Section 3, Disputed Need for Atomic Secrecy, contains papers entitled: Lack of Studies on H-Bomb Proliferation; Administration's Position on H-Bombs; and National Security Needs vs Free Press

  6. Standard methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets

    International Nuclear Information System (INIS)

    Various methods are described in detail as to procedure, interferences, and limits of detection or applicability for the determination of Pu and various impurities in PuO2 powders and pellets. Methods for the determination of Pu are controlled-potential coulometry, ceric sulfate titration, and amperometric titration with Fe2+. Spectrophotometric methods are given for N and S, and a direct combustion-thermal conductivity method for the determination of total C is described. A pyrohydrolysis method is described for the determination of μg amounts of Cl- and F-. A mass spectrometric determination of the Pu isotopic content of the oxide is included, and general chemical methods are included for the determination of moisture in both powders and pellets and for total gas--exclusive of moisture--in pellets. Spectrochemical methods are described for the determination of rare earths, 36 trace elements whose recommended analytical spectral lines and concentration ranges are tabulated, and impurities occurring in the atom-ppB range

  7. Standard test methods for chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1999-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets to determine compliance with specifications. 1.2 This test method covers the determination of uranium and the oxygen to uranium atomic ratio in nuclear-grade uranium dioxide powder and pellets. 1.4 This test method covers the determination of chlorine and fluorine in nuclear-grade uranium dioxide. With a 1 to 10-g sample, concentrations of 5 to 200 g/g of chlorine and 1 to 200 μg/g of fluorine are determined without interference. 1.5 This test method covers the determination of moisture in uranium dioxide samples. Detection limits are as low as 10 μg. 1.6 This test method covers the determination of nitride nitrogen in uranium dioxide in the range from 10 to 250 μg. 1.7 This test method covers the spectrographic analysis of nuclear-grade UO2 for the 26 elements in the ranges indicated in Table 2. 1.8 For simultaneous determination of trace ele...

  8. Aeromagnetic and gamma-ray spectrometric data interpretation for uranium exploration - south eastern margin of the Chattisgarh Basin, India

    International Nuclear Information System (INIS)

    Airborne surveys were conducted along the south-eastern margin of the Chattisgarh Basin - Singhora Basin and Sonakhan greenstone belt by the Atomic Minerals Directorate for Exploration and Research in 2000 with E-W flight lines covering 19800 linekm. Preliminary processed aeromagnetic data were corrected for IGRF, heading and lag and levelled using tie line data. Based on the amplitude, frequency and textural characteristics of enhanced magnetic images, litho-structural information of the area was deciphered. Semi-quantitative interpretation of aeromagnetic data employing Euler's technique facilitated identification of source body locations along with depth estimates. Airborne Gamma Ray Spectrometric (AGRS) data were processed for altitude attenuation, radon interference and stripping corrections. The radiometric ternary image of the processed data shows good correlation with surface geology of the area. Radiometric anomalies were extracted from the derived concentrations based on mean and standard deviation of Uranium, U/Tb and U2/Th data sets. Finally, integrated Geographical Information System (G15) analysis of inferred faults and lineaments from aeromagnetic data and uranium anomalies mapped from AGRS data were used for extracting zones favourable for uranium mineralisation. Qualitative and quantitative analysis of aeromagnetic and AGRS data and integration of the results on a GIS platform thus helped in identifying target areas for further exploration. (author)

  9. 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

  10. 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

  11. 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.

  12. Continuous magnetic trapping of laser cooled atoms

    International Nuclear Information System (INIS)

    The authors present here initial results of the deceleration of a thermal atomic beam from -- 1000 to -- 100 m/s. The experiment was conducted in the 1.4-m long vertical superconducting solenoid which produced the slowing field. The fluorescence of the slowed atomic beam has been studied as a function of laser frequency. Figure 2 is a 12-GHz scan showing the fluorescence at a position 150 cm from the beginning of the solenoid. The wide peak corresponds to unslowed atoms with generally the initial velocity distribution. The second, narrower, peak corresponds to slowed atoms with a velocity of -- 150 m/s. Similar spectra have been obtained for various positions along the magnetic slower and trap. These data should allow better understanding of the cooling process and will be compared to computer models

  13. 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

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

    International Nuclear Information System (INIS)

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

  15. 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...

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

    Science.gov (United States)

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

  17. Determination of Trace Tin in Multimetal Ore by Hydride Generation Atomic Fluorescence Spectrometry%HG-AFS 法测定多金属矿中的痕量锡

    Institute of Scientific and Technical Information of China (English)

    艾军; 周俊明

    2001-01-01

    研究了酒石酸介质中氢化物发生原子荧光光谱法(HG-AFS)测定多金属矿中痕量锡的方法,考察了不同酸介质和浓度对氢化物发生效率的影响,试验了共存元素的干扰情况。方法的检出限为1.4×10-10g/mL,精密度(n=5)为3.71%~5.38%。%A method for determination of trace Sn by hydride generationatomic fluorescence spectrometry (HG-AFS) was described. The influence of HG-AFS operation conditions,various acidic media and concentration of NaBH4 solution was studied.The detection limit is 1.4×10-10 g/mL. The method was applied to determination of trace Sn in the standard multimetal ore samples. The results were in good agreement with certifid values with precision of 3.7%~5.4% RSD(n=5).

  18. Fluorescence correlation spectroscopy

    NARCIS (Netherlands)

    M.A. Hink

    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. Fluorescent optical position sensor

    Science.gov (United States)

    Weiss, Jonathan D.

    2005-11-15

    A fluorescent optical position sensor and method of operation. A small excitation source side-pumps a localized region of fluorescence at an unknown position along a fluorescent waveguide. As the fluorescent light travels down the waveguide, the intensity of fluorescent light decreases due to absorption. By measuring with one (or two) photodetectors the attenuated intensity of fluorescent light emitted from one (or both) ends of the waveguide, the position of the excitation source relative to the waveguide can be determined by comparing the measured light intensity to a calibrated response curve or mathematical model. Alternatively, excitation light can be pumped into an end of the waveguide, which generates an exponentially-decaying continuous source of fluorescent light along the length of the waveguide. The position of a photodetector oriented to view the side of the waveguide can be uniquely determined by measuring the intensity of the fluorescent light emitted radially at that location.

  20. Dielectrophoretic immobilization of proteins: Quantification by atomic force microscopy.

    Science.gov (United States)

    Laux, Eva-Maria; Knigge, Xenia; Bier, Frank F; Wenger, Christian; Hölzel, Ralph

    2015-09-01

    The combination of alternating electric fields with nanometer-sized electrodes allows the permanent immobilization of proteins by dielectrophoretic force. Here, atomic force microscopy is introduced as a quantification method, and results are compared with fluorescence microscopy. Experimental parameters, for example the applied voltage and duration of field application, are varied systematically, and the influence on the amount of immobilized proteins is investigated. A linear correlation to the duration of field application was found by atomic force microscopy, and both microscopical methods yield a square dependence of the amount of immobilized proteins on the applied voltage. While fluorescence microscopy allows real-time imaging, atomic force microscopy reveals immobilized proteins obscured in fluorescence images due to low S/N. Furthermore, the higher spatial resolution of the atomic force microscope enables the visualization of the protein distribution on single nanoelectrodes. The electric field distribution is calculated and compared to experimental results with very good agreement to atomic force microscopy measurements. PMID:26010162

  1. Atomic arias

    Science.gov (United States)

    Crease, Robert P.

    2009-01-01

    The American composer John Adams uses opera to dramatize controversial current events. His 1987 work Nixon in China was about the landmark meeting in 1972 between US President Richard Nixon and Chairman Mao Zedong of China; The Death of Klinghoffer (1991) was a musical re-enactment of an incident in 1985 when Palestinian terrorists kidnapped and murdered a wheelchair-bound Jewish tourist on a cruise ship. Adams's latest opera, Doctor Atomic, is also tied to a controversial event: the first atomic-bomb test in Alamogordo, New Mexico, on 16 June 1945. The opera premièred in San Francisco in 2005, had a highly publicized debut at the Metropolitan Opera in New York in 2008, and will have another debut on 25 February - with essentially the same cast - at the English National Opera in London.

  2. 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.

  3. 流动注射在线离子交换分离富集-氢化物发生原子荧光光谱法测定铜合金中痕量锑%Determination of trace antimony in copper alloys by flow injection on-line ion-exchange separation and enrichment-hydride generation atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    吴良俊; 邱海鸥; 郝志红; 袁红战; 郑洪涛

    2009-01-01

    A method for the determination of trace antimony in copper by flow injection on-line ion-exchange separation and enrichment-hydride generation atomic fluorescence spectrometry is suggested. The manifolds and operating program for ftlow injection on-line ion-exchange were designed and chemical conditions were optimized. Antimony complex was absorbed on strongly basic anion exchange resin 717 with 1. 4 mol/L HC1 as absorbent medium and 2. 0 mol/L HNO_3 for elution. The interference of co-existent elements (i-ron, nickel, lead, etc) was eliminated while antimony was enriched and was determined by hydride generation-atomic fluorescence spectrometry. The method is easy to operate and fast, and has lesser pollution to environment. The linear range is 0. 2-120μg/L and the RSD is 3%~5% with detection limit of 0. 05 μg/L. The results for determination of antimony in standard samples of copper alloys are satisfactory.%提出了流动注射离子交换在线分离富集-氢化物发生原子荧光光谱法测定铜合金中痕量锑的分析方法.设计了流动注射在线离子交换的流路和操作程序,优化了各项化学条件.采用717强碱性阴离子交换树脂吸附锑,并能有效消除铁、镍、铅等元素的干扰,也使大量基体元素铜与待测元素分离,锑在1.4 mol/L的HCl介质中上柱,选用2.0 mol/L的HNO_3作为洗脱剂.实现了氢化物发生原子荧光光谱法对铜合金中痕量锑的在线测定.方法操作简便、快速,环境污染小,线性范围为0.15~120 μg/L,相对标准偏差在3%~5%之间,检出限为0.05μg/L.方法应用于铜合金标准样品,结果与推荐值吻合.

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

    International Nuclear Information System (INIS)

    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

  5. 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

  6. 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.

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

    Science.gov (United States)

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

    2005-05-01

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

  8. 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.

  9. Single shot three-dimensional imaging of dilute atomic clouds

    CERN Document Server

    Sakmann, Kaspar

    2014-01-01

    Light field microscopy methods together with three dimensional (3D) deconvolution can be used to obtain single shot 3D images of atomic clouds. We demonstrate the method using a test setup which extracts three dimensional images from a fluorescent $^{87}$Rb atomic vapor.

  10. 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.

  11. 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.

  12. Application of Hydride Generation-atomic Fluorescence Spectrometry in Determination of Arsenic in Silicon Dioxide in Food Additives%氢化物-原子荧光法在食品添加剂二氧化硅中砷测定的应用

    Institute of Scientific and Technical Information of China (English)

    吴世银

    2012-01-01

    At present, the food additives are the major factor in food industry, but the arsenic and arsenic compounds in the food additive have very strong biological toxicity. So when testing food additives, we should focus on the arsenic element. This article discussed the silicon dioxide as the food additive in food, as well as the basic condition of arsenic in food and summarized the experiment of using the hydride generation-atomic fluorescence spectrometry to determine the arsenic in silicon dioxide in food additives.%目前构成食品工业主要因素就是食品添加剂,但是食品添加剂中砷及砷的化合物有着很强生物毒性.因此对食品添加剂进行检测时,要将检测重点放在砷元素上.本文对食品中作为食品添加剂的二氧化硅以及食品中砷的基本情况进行简单论述,并对应用氢化物-原子荧光法对食品添加剂二氧化硅中微量砷测定的实验进行总结.

  13. 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.

  14. 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

  15. 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.

  16. New FORTRAN computer programs to acquire and process isotopic mass-spectrometric data

    International Nuclear Information System (INIS)

    The computer programs described in New Computer Programs to Acquire and Process Isotopic Mass Spectrometric Data have been revised. This report describes in some detail the operation of these programs, which acquire and process isotopic mass spectrometric data. Both functional and overall design aspects are addressed. The three basic program units - file manipulation, data acquisition, and data processing - are discussed in turn. Step-by-step instructions are included where appropriate, and each subsection is described in enough detail to give a clear picture of its function. Organization of file structure, which is central to the entire concept, is extensively discussed with the help of numerous tables. Appendices contain flow charts and outline file structure to help a programmer unfamiliar with the programs to alter them with a minimum of lost time

  17. Integration of landsat MSS imagery with aeromagnetic and airborne spectrometric data over a part of Mozambique

    International Nuclear Information System (INIS)

    An area within the undifferentiated Precambrian gneisses and granulites of the Mozambique Belt was studied using Landsat MSS imagery, aeromagnetic data and spectrometric data. Airborne radiometric data including total count, uranium, thorium and potassium channels and aeromagnetic data were prepared as raster scanned images, which were registered and combined with the Landsat imagery on an image processing system. In addition to study of the individual data sets the spectrometric channels were manipulated to provide ratios and composite images. These composite images provided information from the three main channels, potassium, uranium and thorium. Single channel images derived from them were colour contoured and integrated with the Landsat imagery. An interpretation of the geophysical data integrated with the Landsat imagery was compared with separate interpretations of each previously carried out. The combined display techniques employed, substantially improved the discrimination of lithology within the area studied and provided a more detailed description of the regional structure. (author). 16 refs, 6 figs, 1 tab

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

    Energy Technology Data Exchange (ETDEWEB)

    Misra, N.L., E-mail: nlmisra@barc.gov.in

    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. - Highlights: • Advantages of TXRF characterization of nuclear materials are described. • The sample amount required/analytical radioactive

  19. 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.

  20. Mass spectrometric analysis of integral membrane proteins: application to complete mapping of bacteriorhodopsins and rhodopsin.

    OpenAIRE

    Ball, L. E.; Oatis, J. E.; Dharmasiri, K.; Busman, M.; Wang, J.; Cowden, L. B.; Galijatovic, A.; N. Chen; Crouch, R K; Knapp, D R

    1998-01-01

    Integral membrane proteins have not been readily amenable to the general methods developed for mass spectrometric (or internal Edman degradation) analysis of soluble proteins. We present here a sample preparation method and high performance liquid chromatography (HPLC) separation system which permits online HPLC-electrospray ionization mass spectrometry (ESI-MS) and -tandem mass spectrometry (MS/MS) analysis of cyanogen bromide cleavage fragments of integral membrane proteins. This method has...

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

    OpenAIRE

    Cai, Min; Liu, Yi-Ming

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-07-01

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

  3. Mass spectrometric analysis of the volatiles released by heating or crushing rocks

    Science.gov (United States)

    Barker, C.; Sommer, M. A.

    1973-01-01

    Vacuum extraction with subsequent mass spectrometric analysis of evolved volatiles was selected as the analytical procedure. The high-vacuum gas-handling system was constructed of stainless steel. The system was completely free from mercury, grease, or volatile organic materials. The furnace for heating the samples is discussed together with the high-vacuum crusher, the mass spectrometer, and approaches for water determination. The analytical procedure is considered, giving attention to the extraction of volatiles, adsorption studies, and the analysis of volatiles.

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

    OpenAIRE

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

    2014-01-01

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

  5. Fluorescent fiber diagnostics

    Science.gov (United States)

    Toeppen, John S.

    1994-01-01

    A fluorescent fiber (13) having a doped core (16) is pumped (11) by light (18) of a relatively short wavelength to produce fluorescence at a longer wavelength that is detected by detector (24). The level of fluorescence is monitored (26) and evaluated to provide information as to the excitation of the fiber (13) or the environment thereof. In particular, the level of intensity of the detected fluorescence may be used to measure the intensity of a light beam (18) passing axially through an optical fiber system (12) (FIG. 1 ), or the intensity of a light beam (46) passing radially through a fluorescent fiber (13) (FIG. 2 ), or the level of a fluid (32) in a tank (31) (FIG. 3 ), or a scintillation event (37) in a fluorescent fiber (13) pumped to produce amplification of the scintillation event (FIG. 4 ).

  6. 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.

  7. Fluorescent minerals, a review

    Science.gov (United States)

    Modreski, P.J.; Aumente-Modreski, R.

    1996-01-01

    Fluorescent minerals are more than just an attractive novelty, and collecting them is a speciality for thousands of individuals who appreciate their beauty, rarity, and scientific value. Fluorescent properties can be used as an aid to mineral identification, locality determination, and distinction between natural and synthetic gemstones. This article gives an overview of those aspects of fluorescence that are of most interest to collectors, hobbyists, and mineralogists. -from Authors

  8. 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.

  9. Laser spectroscopy of sputtered atoms

    International Nuclear Information System (INIS)

    The use of laser radiation to study the sputtering process is of relatively recent origin. Much has been learned from this work about the basic physics of the sputtering process itself through measurements of velocity and excited state distributions of sputtered atoms and the effects of adsorbates on substrate sputtering yields. Furthermore, the identification, characterization, and sensitive detection of sputtered atoms by laser spectroscopy has led to the development of in situ diagnostics for impurity fluxes in the plasma edge regions of tokamaks and of ultrasensitive methods (ppB Fe in Si) for surface analysis with ultralow (picocoulomb) ion fluences. The techniques involved in this work, laser fluorescence and multiphoton resonance ionization spectroscopy, will be described and illustrations given of results achieved up to now. 55 refs., 5 figs., 1 tab

  10. Detection of terrestrial radionuclides with X-ray fluorescence analysis.

    Science.gov (United States)

    Trojek, T; Čechák, T

    2015-06-01

    This paper provides an overview of analytical methods frequently used to identify terrestrial radionuclides in samples. While radioactivity is normally measured through the ionising radiation produced during the spontaneous decay of unstable atoms, selected radionuclides or their chemical elements can be quantified with instrumental techniques based on stimulated emission or counting of atoms. The advantages and disadvantages of these analytical methods are discussed. Particular attention is paid to X-ray fluorescence analysis of materials containing uranium and thorium. It is also possible to determine the area distributions of these chemical elements in samples with the use of scanning X-ray fluorescence systems. PMID:25977354

  11. Fluorescence in insects

    Science.gov (United States)

    Welch, Victoria L.; Van Hooijdonk, Eloise; Intrater, Nurit; Vigneron, Jean-Pol

    2012-10-01

    Fluorescent molecules are much in demand for biosensors, solar cells, LEDs and VCSEL diodes, therefore, considerable efforts have been expended in designing and tailoring fluorescence to specific technical applications. However, naturally occurring fluorescence of diverse types has been reported from a wide array of living organisms: most famously, the jellyfish Aequorea victoria, but also in over 100 species of coral and in the cuticle of scorpions, where it is the rule, rather than the exception. Despite the plethora of known insect species, comparatively few quantitative studies have been made of insect fluorescence. Because of the potential applications of natural fluorescence, studies in this field have relevance to both physics and biology. Therefore, in this paper, we review the literature on insect fluorescence, before documenting its occurrence in the longhorn beetles Sternotomis virescens, Sternotomis variabilis var. semi rufescens, Anoplophora elegans and Stellognatha maculata, the tiger beetles Cicindela maritima and Cicindela germanica and the weevil Pachyrrhynchus gemmatus purpureus. Optical features of insect fluorescence, including emitted wavelength, molecular ageing and naturally occurring combinations of fluorescence with bioluminescence and colour-producing structures are discussed.

  12. 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

  13. 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

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

    International Nuclear Information System (INIS)

    Inexpensive baker's yeast Saccharomyces cerevisiae and green algae Chlorella vulgaris, either free or immobilized on silica gel have been shown to selectively accumulate platinum and palladium from water samples in acidic medium (pH 1.6-1.8). Optimization of conditions of metals biosorption (sample pH, algae and yeast masses, adsorption time, temperature) was performed in batch mode. The procedure of matrix separation based on biosorption of platinum and palladium on algae C. vulgaris covalently immobilized on silica gel in flow mode was developed. The use of algae in flow procedure offers several advantages compared with its use in the batch mode. The procedure shows better reproducibility (-1 thiourea in 1 mol l-1 hydrochloric acid. The influence of thiourea on analytical signals of examined metals during GFAAS determination is discussed. The procedure has been applied for separation of noble metals from tap and waste water samples spiked with platinum and palladium

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

    International Nuclear Information System (INIS)

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

  16. 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

    ... in Academic Chemistry Laboratories, American Chemical Society Publication, Committee on Chemical..., Publication No. 77-206, August 1977. 14.8“OSHA Safety and Health Standards, General Industry,” (29 CFR part... been precisely defined; however, each chemical compound should be treated as a potential health...

  17. 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.

  18. 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%.

  19. Determination of Trace Inorganic Mercury in Mineral Water by Flow Injection On-line Sorption Preconcentration-Cold Vapor Atomic Fluorescence Spectrometry%流动注射在线吸附预富集-冷蒸气原子荧光法测定矿泉水中的痕量无机汞

    Institute of Scientific and Technical Information of China (English)

    訾洪静; 淦五二; 韩素平; 姜宪娟; 完玲中

    2009-01-01

    Flow injection on-line sorption preconcentration and separation in a knotted reactor (KR) was coupled to cold vapor atomic fluorescence spectrometry for the determination of trace mercury in mineral water. Mercury was preconcentrated by on-line formation of mercury diethyldithiocarbamate complex (Hg-DDTC) and absorption of the resulting neutral complex on the inner walls of a knotted reactor. A 20%(V/V) HNO3 solution heated by electromagnetic induction heating technique was used as eluent to remove the absorbed Hg-DDTC from the KR, and then the vapor mercury generated by mixing the resulting solution and KBH4 was determined on-line by cold vapor atomic fluorescence spectrometry. The 20% HNO3 was employed as both the efficient eluent and the required acidic medium for subsequent mercury vapor generation in our work. Using 20% HNO3 instead of conventional organic solvent as eluent, the proposed method is simple, easy operational and environmentally friendly. Under the optimal experimental conditions, the sample throughput was approximatively 30/h with an enhancement factor of 35. The detection limit of mercury was 2.0 ng/L. The precision(RSD, n=11) was 2.2% at the 0.1 μg/L Hg2+ level.%研究了聚四氟乙烯管编结反应器(KR)在线吸附预富集技术与冷蒸气原子荧光联用测定矿泉水中痕量无机汞的方法.Hg2+与DDTC在线形成Hg2+-DDTC络合物并吸附在KR内壁上,采用电磁感应加热技术,用20% (V/V) HNO3在线加热洗脱并氧化预富集于KR内壁上的Hg2+-DDTC.洗脱液与KBH4溶液反应生成蒸气态汞,直接用冷蒸气原子荧光联用技术检测.20%(V/V)HNO3作为洗脱液的同时也为氢化发生提供了酸性介质.本方法未使用常用的有机洗脱液,具有操作简单和环保等优点.每小时可分析30个样品,最大吸附倍数为35倍,样品分析精密度RSD为2.2%(n=11),检出限(3σ)为2.0 ng/L.

  20. 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.

  1. Atom trapping in a bottle beam created by a diffractive optical element

    CERN Document Server

    Ivanov, V V; Saffman, M; Kemme, S A; Ellis, A R; Brady, G R; Wendt, J R; Biedermann, G W; Samora, S

    2013-01-01

    A diffractive optical element (DOE) has been fabricated for creating blue detuned atomic bottle beam traps. The DOE integrates several diffractive lenses for trap creation and imaging of atomic fluorescence. We characterize the performance of the DOE and demonstrate trapping of cold Cesium atoms inside a bottle beam.

  2. 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)

  3. 氢化物发生-原子荧光光谱法同时测定红土镍矿中砷锑铋%Determination of arsenic,antimony and bismuth in laterite nickel ore by hydride generation-atomic fluorescence spectrometry

    Institute of Scientific and Technical Information of China (English)

    何飞顶; 李华昌; 袁玉霞

    2011-01-01

    The content of arsenic,antimony and bismuth in laterite nickel ore was determined with hydride generation-atomic fluorescence spectrometry( HG-AFS). The influencing factors were discussed in detail. The aqua regia bath was adopted for reducing the volatile loss of elements to be tested,while the mixed solution of thiourea and ascorbic acid was used as masking reagent to eliminate the impact of interfering elements. The detection limit of method was between 0. 10-0. 25 ng/mL. The arsenic,antimony and bisnmuth in laterite nickel ore was analyzed with the recovery of 91%-113% and relative standard deviation( RSD) of 1. 9 %-7. 6 %.%采用氢化物发生-原子荧光光谱(HG-AFS)法测定红土镍矿中砷、锑、铋含量,并对影响其光谱测量的各种因素进行了较为详细的探讨.实验中,以王水水浴法溶解样品降低待测元素的挥发损失,以硫脲和抗坏血酸混合溶液为掩蔽剂来消除干扰元素的影响.方法的检出限在0.10~0.25 ng/mL之间;对红土镍矿样品中的砷、锑、铋进行分析,其回收率在91%~113%之间,相对标准偏差(RSD)为1.9%~7.6%.

  4. Study on simultaneous determination of Bi and Hg in chinese herbal medicine by the sequential injection hydride generation atomic fluorescence spectrometry%顺序注射氢化物发生-原子荧光光谱法同时测定中草药中铋和汞

    Institute of Scientific and Technical Information of China (English)

    徐文军

    2009-01-01

    建立了一种顺序注射氢化物发生-原子荧光光谱法测定中草药中的Bi和Hg的方法, 讨论了共存离子的干扰情况. 在最佳实验条件下, Bi和Hg的检出限分别为0.0057 μg/L和0.0197 μg/L, 加标回收率为93.4%~104.7%, 相对标准偏差小于4.3%, 被测中草药试样中共存的离子对Bi和Hg的测定没有干扰. 方法可用于中草药试样中Bi和Hg的同时测定.%A method for the determination of Bi and Hg in Chinese herbal medicine by sequential injection hydride generation atomic fluorescence spectrometry was established. The interference circumstance of the coexistence ions at the same time was discussed. Under the proposed conditions, the detection limits of the Bi and Hg were 0.0057 and 0.0197 μg/L. Recoveries of standard addition of the Bi and Hg have been proveed to be 93.4% ~104.7% in samples . The maximum RSD was 4.3%. The coexistence ions in chinese herbal medicine samples hardly interfered in the determination of bismuth and mercury. The operation was easy and its sensitivity was high. This method is feasible and practicable to determine bismuth and mercury in chinese herbal medicine.

  5. 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.

  6. "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…

  7. 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.

  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. Analysis of a single-atom dipole trap

    International Nuclear Information System (INIS)

    We describe a simple experimental technique which allows us to store a single 87Rb atom in an optical dipole trap. Due to light-induced two-body collisions during the loading stage of the trap the maximum number of captured atoms is locked to one. This collisional blockade effect is confirmed by the observation of photon antibunching in the detected fluorescence light. The spectral properties of single photons emitted by the atom were studied with a narrow-band scanning cavity. We find that the atomic fluorescence spectrum is dominated by the spectral width of the exciting laser light field. In addition we observe a spectral broadening of the atomic fluorescence light due to the Doppler effect. This allows us to determine the mean kinetic energy of the trapped atom corresponding to a temperature of 105 μK. This simple single-atom trap is the key element for the generation of atom-photon entanglement required for future applications in quantum communication and a first loophole-free test of Bell's inequality

  10. Energetics and dynamics of atomic uranium levels

    International Nuclear Information System (INIS)

    New methods for discovering and identifying new electronic levels of atomic uranium and measuring parameters, such as radiative lifetimes and absorption cross-sections, are described. The uranium atoms are produced within an especially designed induction-heated oven. The uranium vapor is irradiated by nitrogen laser pumped, pulsed dye lasers. The various measurements are accomplished by detection of laser induced fluorescence from selectively excited levels. 138 atomic-uranium odd levels in the region 32260-34900 cm-1 and 16 even levels in the region 49500-49900 cm-1 are reported. Unique J values are presented for 64 levels and partial assignment (two possibilities) for 42 levels. Radiative lifetimes are presented for 134 levels. Absorption cross sections were measured for 12 transitions. Isotope shifts of 17 levels are given. Cross-sections for internal excitation transfer in uranium which are induced by collisions with argon atoms, are presented for 11 levels. (author)

  11. A quantum gas microscope for ytterbium atoms

    Science.gov (United States)

    Takahashi, Yoshiro

    2016-05-01

    In this talk, I report on the development of a quantum gas microscope for ytterbium (Yb) atoms. By using a dual molasses technique in which 399 nm molasses beams of the broad singlet transition are applied for fluorescence imaging and 556 nm molasses beams of the narrow intercombination transition are applied for cooling during the imaging, we successfully demonstrate site-resolved imaging of individual bosonic 174 Yb atoms in a two-dimensional optical lattice with a lattice constant of 266 nm.We also apply a high resolution laser spectroscopy using the ultranarrow intercombination transition between the 1 S0 and 3 P2 states to manipulate an atom distribution in an optical lattice. We expect the demonstrated technique will similarly work for other isotopes of Yb atoms. We are also developing a different mode of an Yb quantum gas microscope.

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

    DEFF Research Database (Denmark)

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

    2013-01-01

    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...

  13. 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.

  14. Atomic Energy Basics, Understanding the Atom Series.

    Science.gov (United States)

    Atomic Energy Commission, Oak Ridge, TN. Div. of Technical Information.

    This booklet is part of the "Understanding the Atom Series," though it is a later edition and not included in the original set of 51 booklets. A basic survey of the principles of nuclear energy and most important applications are provided. These major topics are examined: matter has molecules and atoms, the atom has electrons, the nucleus,…

  15. Teach us atom structure

    International Nuclear Information System (INIS)

    This book is written to teach atom structure in very easy way. It is divided into nine chapters, which indicates what is the components of matter? when we divide matter continuously, it becomes atom, what did atom look like? particles comprised of matter is not only atom, discover of particles comprised of atom, symbol of element, various radiation, form alchemy to nuclear transmutation, shape of atom is evolving. It also has various pictures in each chapters to explain easily.

  16. Teach us atom structure

    Energy Technology Data Exchange (ETDEWEB)

    Lim, Suh Yeon

    2006-08-15

    This book is written to teach atom structure in very easy way. It is divided into nine chapters, which indicates what is the components of matter? when we divide matter continuously, it becomes atom, what did atom look like? particles comprised of matter is not only atom, discover of particles comprised of atom, symbol of element, various radiation, form alchemy to nuclear transmutation, shape of atom is evolving. It also has various pictures in each chapters to explain easily.

  17. 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.

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

    International Nuclear Information System (INIS)

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

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

    Science.gov (United States)

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

    2009-07-01

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

  20. Mass spectrometric studies on irradiated (U, Pu) mixed carbide fuel of Fbtr

    Energy Technology Data Exchange (ETDEWEB)

    Balasubramanian, R. [Fuel Chemistry Division, IGCAR, Kalpakkam 603 102, Tamil Nadu (India)]. E-mail: rbs@igcar.ernet.in; Darwin Albert Raj, D.; Nalini, S.; Sai Baba, M. [Fuel Chemistry Division, IGCAR, Kalpakkam 603 102, Tamil Nadu (India)

    2005-07-01

    Mass spectrometry was employed to characterise the irradiated mixed carbide fuel of fast breeder test reactor (FBTR) for assessing its performance: thermal ionisation mass spectrometry to determine the isotopic composition, concentrations of U, Pu and Nd in the dissolver solutions and to deduce the burn-up, and a quadrupole mass spectrometric system to obtain the percentage release of fission gases (Kr + Xe). A summary and analysis of the results obtained with the fuel at 25,000 and 50,000 MWd/t in these studies is given in this paper. (author)

  1. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade boron carbide

    Energy Technology Data Exchange (ETDEWEB)

    1981-01-01

    The standard covers analytical procedures to determine compliance of nuclear-grade boron carbide powder and pellets to specifications. The following methods are described in detail: total carbon by combustion and gravimetry; total boron by titrimetry; isotopic composition by mass spectrometry; chloride and fluoride separation by pyrohydrolysis; chloride by constant-current coulometry; fluoride by ion-selective electrode; water by constant-voltage coulometry; impurities by spectrochemical analysis; soluble boron by titrimetry; soluble carbon by a manometric measurement; metallic impurities by a direct reader spectrometric method. (JMT)

  2. Fluorescent filtered electrophosphorescence

    Science.gov (United States)

    Forrest, Stephen R.; Sun, Yiru; Giebink, Noel; Thompson, Mark E.

    2009-01-06

    The present invention relates to organic light emitting devices (OLEDs), and more specifically to OLEDS that emit light using a combination of fluorescent emitters and phosphorescent emitters for the efficient utilization of all of the electrically generated excitons.

  3. 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

  4. 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.

  5. Resonance Fluorescence in Two-Photon JC Models Analyzed by Supersymmetric Transformation

    Institute of Scientific and Technical Information of China (English)

    LIANG Xian-Ting; SUN Ming-Zhai

    2002-01-01

    Resonance fluorescences of two-photon two-level and two-photon three-level atoms driven by laser are investigated with supersymmetric transformation.It is shown that the spectrum of fluorescent light obtained from the supersymmetric transformation is more accurate and the physical process shown by this method is clearer than that from dress transformation.

  6. HF Fluorescence and Ion Production From Infrared Laser Irradiation of SF6-Hydrocarbon Mixtures

    OpenAIRE

    Scypinski, S.; Kaldor, A.; Cox, D.M.

    1984-01-01

    CO2 laser irradiation of SF6/hydrocarbon mixtures are shown to produce positive ions and infrared fluorescence due to emission by HF≠. The mechanism for the production of these ions and fluorescence involves the multiple photon dissociation of SF6 and subsequent attack of the free fluorine atom on the hydrocarbon, as well as V → V transfer and thermal ionization reactions. Argon and oxygen are found to increase ion production while quenching the fluorescence. Chemi-ionization of the hydrocarb...

  7. Pattern formation of quantum jumps with Rydberg atoms

    CERN Document Server

    Lee, Tony E

    2012-01-01

    We study the nonequilibrium dynamics of quantum jumps in a one-dimensional chain of atoms. Each atom is driven on a strong transition to a short-lived state and on a weak transition to a metastable state. We choose the metastable state to be a Rydberg state so that when an atom jumps to the Rydberg state, it inhibits or enhances jumps in the neighboring atoms. This leads to rich spatiotemporal dynamics that are visible in the fluorescence of the strong transition. It also allows one to dissipatively prepare Rydberg crystals.

  8. 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.

  9. Determination of Trace Selenium in Plants by Hydride Generation Atomic Fluorescence Spectrometry with Program Temperature- Controlled Graphite Digestion%程序控温石墨消解-氢化物原子荧光光谱法测定植物中痕量硒

    Institute of Scientific and Technical Information of China (English)

    钱薇; 蒋倩; 王如海; 龚华; 韩勇

    2014-01-01

    Discussed several methods of pretreatment for the determination of selenium were discussed ,and a program tempera-ture-controlled graphite digestion method was developed to digest 5 kinds of representative standard plant samples of citrus leav-es ,tea ,cabbage leaves ,shrubs and rice .The effect of the pretreatment method of digestion solution ,digestion temperature and digestion time on the extraction of selenium was investigated in detail .The instrumental working parameters were optimized .For the reaction conditions of hydride generation atomic fluorescence spectrometry (HG-AFS) ,the effect of the concentration of KBH4 and HCl on the determination of selenium was emphasized .Not only the effect of the concentration of carrier fiow HCl was considered ,but also the effect of the concentration of sample HCl on the determination of selenium was studied .The best method for determination of trace selenium in plant samples by atomic fluorescence spectrometry with program temperature-con-trolled graphite digestion was established .Results indicated that the recovery of the method of selenium was 87.1% ~106 .2% , the detection limit was 0.018 μg · L -1 and the relative standard deviation (RSD) was less than 6.0% .In the range of 0~10 μg · L -1 (low standard) and 0~100μg · L -1 (high standard) fluorescence was linearly related to the concentration of selenium ,the coefficient of r was 0.999 9 and r was 0.999 7 .Therefore ,this method has wide linear range ,high sensitivity ,low detection limit and good stability ,which was very suitable for the determination of trace selenium of plant .And the method was of easy and safe operation ,strong practicability ,low cost ,and low toxicity of chemicals used ,so it can be used as a routine analysis method in general laboratory .%探讨了硒测定的几种预处理方法,采用一种程序控温的石墨消解系统来消化处理柑橘叶、茶叶、灌木叶、圆白菜、大米五种代表性的植物标准样品。

  10. Atomic transition probabilities of neutral samarium

    International Nuclear Information System (INIS)

    Absolute atomic transition probabilities from a combination of new emission branching fraction measurements using Fourier transform spectrometer data with radiative lifetimes from recent laser induced fluorescence measurements are reported for 299 lines of the first spectrum of samarium (Sm i). Improved values for the upper and lower energy levels of these lines are also reported. Comparisons to published transition probabilities from earlier experiments show satisfactory and good agreement with two of the four published data sets. (paper)

  11. Arsenic and antimony determination in refined and unrefined table salts by means of hydride generation atomic absorption spectrometry--comparison of sample decomposition and determination methods

    OpenAIRE

    AKSUNER, Nur; TİRTOM, Vedia Nüket; HENDEN, Emür

    2011-01-01

    An evaluation was made of different digestion methods for the determination of arsenic and antimony in table salt samples prior to hydride generation atomic absorption spectrometric analysis. Microwave acid digestion, classical wet digestion, dry ashing, and fusion were applied to the decomposition of salt samples and optimum conditions were investigated. Samples were decomposed by changing heating time, digestion techniques, and the amount and composition of acid, and then the concen...

  12. 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.

  13. 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.

  14. 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.

  15. Determination of trace quantities of uranium in rocks mass spectrometric isotope dilution technique

    International Nuclear Information System (INIS)

    A detailed experimental investigation on the thermionic emission of uranium deposited on a single flat type rhenium filament has been carried out. The study was aimed at determining the influence of various forms of deposition on the emission sensitivity and thermal stability of U+ , UO+ and UO2+ ions. Based on these investigations, a technique, involving an addition of a small quantity of colloidal suspension of graphite on top of the uranyl nitrate sample deposited, was chosen because of its higher, emission sensitivity for uranium metal ions. The experimental parameters of the technique were optimised and the technique was employed in the determination of trace quantities of uranium in rock samples using mass spectrometric isotope dilution method. For the mass spectrometric isotope dilution analysis National Bureau of Standards uranium isotopic standard NBS-U 970 was employed as a tracer, where as the mass discrimination effect in the uranium isotope analysis was corrected using the uranium isotopic standard NBS-U500. Uranium was determined in each of the seven granite samples from Wyoming, USA and two USGS standard rocks. The precision of the analysis was found to be ±1% . The uranium values obtained on the rock samples were compared with the analyses of other investigators. Influence of the sample splitting on the uranium analysis was discussed in the light of the analytical results obtained.(author)

  16. MALDI mass spectrometric imaging meets "omics": recent advances in the fruitful marriage.

    Science.gov (United States)

    Crecelius, A C; Schubert, U S; von Eggeling, F

    2015-09-01

    Matrix-assisted laser desorption/ionization mass spectrometric imaging (MALDI MSI) is a method that allows the investigation of the molecular content of surfaces, in particular, tissues, within its morphological context. The applications of MALDI MSI in the field of large-scale mass spectrometric studies, which are typically denoted by the suffix "omics", are steadily increasing. This is because, on the one hand, technical advances regarding sample collection and preparation, matrix application, instrumentation, and data processing have enhanced the molecular specificity and sensitivity of MALDI MSI; on the other hand, the focus of the "omics" community has moved from establishing an inventory of certain compound classes to exploring their spatial distribution to gain novel insights. Thus, the aim of this mini-review is twofold, to display the state-of-the-art in terms of technical aspects in MALDI MSI and to highlight selected applications in the last two years, which either have significantly advanced a certain "omics" field or have introduced a new one through pioneering efforts. PMID:26161715

  17. New miniaturized alpha/beta spectrometric systems for the surface contamination monitoring and radon personal dosimeter

    International Nuclear Information System (INIS)

    We report on a new miniaturized alpha/beta spectrometric system. This cheque cart 12 bit SARAD spectra 5011 spectrometric system we can combine with a new developed detector, preamp and forming unit. A very important application of this new measuring system is the alpha nuclidspecific surface contamination monitoring. Especially in old nuclear power station it is very important in the decommissioning process to know the nuclide vector. We report of applications to use this new technology to measure the nuclide vector in old lead cells or construction elements in old nuclear reactors. We measure surface contamination in the order of 1 Bq/cm2 of Pu-239 very easy. A other modification of this cheque cart spectrometer is the radon personal dosimeter. In this case we have integrated on a cheque cart a 8 bit spectrometer, a 1cm2 silicon detector, the signal processing, AD-conversion, data storage and transponder system for the data transfer. Using this transponder system we can also use a local resoluted dosimetry. The main application of this system is the radon dosimetry on workplaces, for instance water works, mines, show caves and other work places with high radon levels. This easy system can replace the passive screening methods and also the nuclear track etch dosimeters. Because the low price and the easy data read out the amortisation of such a electronic system is in the order of two years

  18. Particle size independent spectrometric determination of wear metals in aircraft lubricating oils

    International Nuclear Information System (INIS)

    A method for the particle size independent determination of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti in synthetic ester lubricating oils by spectrometric analysis is presented. Partial dissolution of Cr, Si, Pb, and Ag also occurs. Used ester lubricating oils as well as samples prepared with -325 mesh (44 μm) or -200 mesh (74 μm) metal powders were reacted with a small amount of hydrofluoric acid and aqua regia at 650C for 45 min with ultrasonic agitation. The reacted mixture was then diluted with a methyl isobutyl ketone and isopropyl alcohol mixture and analyzed spectrometrically. The recoveries for metal powder suspensions of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti ranged from 97 to 103% and the relative standard deviation ranged from 4 to 10%. In addition to the metal powder suspensions, over 200 aircraft oil samples were analyzed. The method is much faster and more convenient than previously reported particle size independent methods using ashing techniques

  19. The determination of trace metals in lubricating oils by atomic spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Aucelio, Ricardo Q. [Departamento de Quimica, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente 225, 22451-900 Rio de Janeiro (Brazil)], E-mail: aucelior@rdc.puc-rio.br; Martins de Souza, Roseli; Calixto de Campos, Reinaldo; Miekeley, Norbert; Porto da Silveira, Carmem L. [Departamento de Quimica, Pontificia Universidade Catolica do Rio de Janeiro, Rua Marques de Sao Vicente 225, 22451-900 Rio de Janeiro (Brazil)

    2007-09-15

    The determination of trace metals in lubricating oils using atomic spectrometric methods is reviewed. The importance of such analyses for technical diagnostics as well as the specific sample characteristics related to the analyte form (metallo-organic and metal particles) is discussed. Problems related to sample pre-treatment for appropriate sample introduction and calibration are addressed as well as the strategies to overcome them. Recent trends aimed at simplifying sample manipulation are presented. The applications and scope of AAS, ICP OES and ICP MS techniques for the determination of trace metals in lubricating oil is individually discussed, as well as some present instrumental trends.

  20. Equipment and dosimetry for radiobiological experiments with the IRT-2000 atomic reactor. [Survival of mice

    Energy Technology Data Exchange (ETDEWEB)

    Voskresenskii, V.V.; Mikhailov, A.L.; Litskevich, L.A.; Stukanov, S.L.; Dokshina, G.A.

    1977-01-01

    A description is given of the distinctive features of design and equipment of the biological channel of the IRT-2000 atomic reactor. A study was made of spectrometric and dosimetric characteristics of a guided (''channeled'') beam of mixed gamma and neutron radiation. It was demonstrated that mixed gamma and neutron fields can be obtained with virtually any contribution of neutron component to the total dose. Determination was made of survival of mice exposed to gamma and neutron fields varying in dosage of each component.

  1. ALPHA SPECTROMETRIC EVALUATION OF SRM-995 AS A POTENTIAL URANIUM/THORIUM DOUBLE TRACER SYSTEM FOR AGE-DATING URANIUM MATERIALS

    Energy Technology Data Exchange (ETDEWEB)

    Beals, D.

    2011-12-06

    Uranium-233 (t{sub 1/2} {approx} 1.59E5 years) is an artificial, fissile isotope of uranium that has significant importance in nuclear forensics. The isotope provides a unique signature in determining the origin and provenance of uranium-bearing materials and is valuable as a mass spectrometric tracer. Alpha spectrometry was employed in the critical evaluation of a {sup 233}U standard reference material (SRM-995) as a dual tracer system based on the in-growth of {sup 229}Th (t{sub 1/2} {approx} 7.34E3 years) for {approx}35 years following radiochemical purification. Preliminary investigations focused on the isotopic analysis of standards and unmodified fractions of SRM-995; all samples were separated and purified using a multi-column anion-exchange scheme. The {sup 229}Th/{sup 233}U atom ratio for SRM-995 was found to be 1.598E-4 ({+-} 4.50%) using recovery-corrected radiochemical methods. Using the Bateman equations and relevant half-lives, this ratio reflects a material that was purified {approx} 36.8 years prior to this analysis. The calculated age is discussed in contrast with both the date of certification and the recorded date of last purification.

  2. Identification strategy using combined mass spectrometric techniques for elucidation of phase I and phase II in vitro metabolites of lipophilic marine biotoxins.

    Science.gov (United States)

    Kittler, Katrin; Preiss-Weigert, Angelika; These, Anja

    2010-11-15

    Combining mass spectrometric tools, a total of 47 in vitro metabolites of okadaic acid (OA), dinophysistoxins 1 and 2 (DTX1 and DTX2), yessotoxin (YTX), azaspiracid1 (AZA1), and pectenotoxin 2 (PTX2) could be detected and confirmed after an incubation with rat liver S9-mix. In a first step, liquid chromatography (LC) combined with tandem mass spectrometry (MS/MS) was used as a screening tool for the identification of in vitro metabolites of lipophilic marine biotoxins. Metabolic phase I and phase II reactions were screened for metabolites by calculating and subsequently monitoring theoretical MS transitions. In a second step, metabolites were confirmed by determination of accurate masses using high resolution MS provided by Orbitrap technology. Subsequently, product ion spectra, precursor ion spectra, and MS3 spectra were recorded for structure elucidation of metabolites. While all investigated toxins were found to form various oxygenated metabolites during the oxidative phase I metabolism, those metabolites varied in the number of added oxygen atoms and in the number of individual isomers. No hints were obtained concerning the formation of glutathione adducts, and a conjugation with glucuronic acid was detected for AZA1 only.

  3. Fluorescent image tracking velocimeter

    Science.gov (United States)

    Shaffer, Franklin D.

    1994-01-01

    A multiple-exposure fluorescent image tracking velocimeter (FITV) detects and measures the motion (trajectory, direction and velocity) of small particles close to light scattering surfaces. The small particles may follow the motion of a carrier medium such as a liquid, gas or multi-phase mixture, allowing the motion of the carrier medium to be observed, measured and recorded. The main components of the FITV include: (1) fluorescent particles; (2) a pulsed fluorescent excitation laser source; (3) an imaging camera; and (4) an image analyzer. FITV uses fluorescing particles excited by visible laser light to enhance particle image detectability near light scattering surfaces. The excitation laser light is filtered out before reaching the imaging camera allowing the fluoresced wavelengths emitted by the particles to be detected and recorded by the camera. FITV employs multiple exposures of a single camera image by pulsing the excitation laser light for producing a series of images of each particle along its trajectory. The time-lapsed image may be used to determine trajectory and velocity and the exposures may be coded to derive directional information.

  4. 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%。

  5. Determination of arsenic in bag tea samples of health food by hydride generator atomic fluorescence spectrometry%氢化物发生-原子荧光光度法测定保健食品袋泡茶中的总砷

    Institute of Scientific and Technical Information of China (English)

    王正; 张妮娜; 李敏; 沙博郁; 罗仁才

    2011-01-01

    Objective: To establish a method of hydride generator atomic fluorescence spectrometry ( HG - AFS) to determine arsenic in bag tea samples of 20 kinds of health food. Methods: After microwave or wet digestion, the contents of arsenic in twenty bag tea samples were determined by HG - AFS. Results: Linear range for the determination of arsenic was 0 |xg/L ~ 80 μg/L. The linear correlative coefficient for arsenic was 0.9994. The quality of the results was proved by the recovery experiments ( ranging from 92.4% to 109.6% ). The relative standard deviation was 2.5% (n = 11) for arsenic in bag tea samples. The contents of arsenic in bag tea were in the range of 0.10 mg/kg ~0.80 mg/kg. Conclusion: The findings indicate that the proposed method is simple, fast and accurate, which can meet the demand for determining arsenic in bag tea samples of health food.%目的:本文建立了保健食品袋泡茶中总砷的测定方法并测定了20种保健食品袋泡茶中总砷含量.方法:以微波消解和湿消解法处理样品,原子荧光光度法进行测定.结果:本文测定总砷的线性范围为0 μg/L~80μg/L,相关系数为0.9994,方法回收率为92.4%~109.6%,RSD为2.5%.测定的20种保健食品袋泡茶中总砷含量为0.10 mg/kg~0.80 mg/kg.结论:实验表明,本法简单、快速、准确,可以用于保健食品袋泡茶中总砷含量的测定.

  6. Microwave digestion-hydride generation-atomic fluorescence spectrometry determination of arsenic and mercury in imported copper matte%微波消解一氢化物发生原子荧光光谱法测定进口铜锍中砷和汞

    Institute of Scientific and Technical Information of China (English)

    葛钰玮; 索金玲; 王成; 胡晓民

    2011-01-01

    A determination method of arsenic and mercury in imported copper mattc by hydride generation- atomic fluorescence spectrometry (AFS) was established. The copper matte samples were digested in aqua regia and hydrofluoric acid by microwave. Then, the solution was diluted. The thiourea and ascorbic acid were added into digestion solution for prereduction Arsenic and mercury were made to form hydride by adding potassium borohydride. The contents of arsenic and mercury were determined by AFS. The results indicated that the matrix effect of Cu, Fe and S on the determination of elements was not obvious. Under the selected conditions, the detection limits were for arsenic and mercury were 0. 003 9 μg/L and 0. 060 8 μg/L, respectively. The recoveries of standard addition were 95 %-123%, and the relative standard deviations (RSD, n=10) were 0. 56 % and 2. 0% for arsenic and mercury, respectively. The proposed method could be used for the determination of arsenic and mercury in large quantities of copper matte samples.%建立了测定进口铜锍样品中砷、汞含量的氢化物发生原子荧光光谱法.在铜锍试样中加入王水和氢氟酸,经微波消解后稀释,消解液中加入硫脲-抗坏血酸预还原,加硼氢化钾使砷和汞生成硼氢化物,用原子荧光光谱法测定砷和汞含量.铜、铁、硫等对待测元素基体效应不显著.在选定条件下,砷和汞的检出限分别为0.003 9μg/L和0.060 8μg/L,样品的加标回收率在95%~123%之间,砷和汞的相对标准偏差分别为0.56%和2.0%(n=6),方法可用于大批铜锍样品中砷和汞的测定.

  7. MULTIPHOTON IONIZATION OF ATOMS

    OpenAIRE

    Mainfray, G.

    1985-01-01

    Multiphoton ionization of one-electron atoms, such as atomic hydrogen and alkaline atoms, is well understood and correctly described by rigorous theoretical models. The present paper will be devoted to collisionless multiphoton ionization of many-electron atoms as rare gases. It induces removal of several electrons and the production of multiply charged ions. Up to Xe5+ ions are produced in Xe atoms. Doubly charged ions can be produced, either by simultaneous excitation of two electrons, or b...

  8. Stable atomic hydrogen: Polarized atomic beam source

    International Nuclear Information System (INIS)

    We have carried out experiments with stable atomic hydrogen with a view to possible applications in polarized targets or polarized atomic beam sources. Recent results from the stabilization apparatus are described. The first stable atomic hydrogen beam source based on the microwave extraction method (which is being tested ) is presented. The effect of the stabilized hydrogen gas density on the properties of the source is discussed. (orig.)

  9. Dynamics Resonances in Atomic States of Astrophysical Relevance

    Indian Academy of Sciences (India)

    K. N. Arefieff; K. Miculis; N. N. Bezuglov; M. S. Dimitrijević; A. N. Klyucharev; A. A. Mihajlov; V. A. Srećković

    2015-12-01

    Ionized geocosmic media parameters in a thermal and a subthermal range of energy have a number of unique features. The photoresonance plasma that is formed by optical excitation of the lowest excited (resonance) atomic states is one example of conversion of radiation energy into electrical one. Since spontaneous fluorescence of excited atoms is probabilistic, the description of the radiating quantized system evolution along with photon energy transfer in a cold atom medium, should include elements of stochastic dynamics. Finally, the chaotic dynamics of a weakly bound Rydberg electron over a grid of the energy level diagram of a quasi-molecular Rydberg complex provides an excitation migration of the electron forward to the ionization continuum. This work aims at discussing the specific features of the dynamic resonances formalism in the description of processes involving Rydberg states of an excited atom, including features in the fluorescence spectrum partially caused by the quantum defect control due to the presence of statistic electromagnetic fields.

  10. Dynamics Resonances in Atomic States of Astrophysical Relevance

    CERN Document Server

    Arefieff, K N; Bezuglov, N N; Dimitrijevic, M S; Klyucharev, A N; Mihajlov, A A; Sreckovic, V A

    2016-01-01

    Ionized geocosmic media parameters in a thermal and a subthermal range of energy have a number of unique features. The photoresonance plasma that is formed by optical excitation of the lowest excited (resonance) atomic states is one example of conversion of radiation energy into electrical one. Since spontaneous fluorescence of excited atoms is probabilistic, the description of the radiating quantized system evolution along with photons energy transfer in a cold atoms medium, should include elements of stochastic dynamics. Finally, the chaotic dynamics of a weakly bound Rydberg electron over a grid of the energy levels diagram of a quasi-molecular Rydberg complex provides an excitation migration of the electron forward to the ionization continuum. This work aims at discussing the specific features of the dynamic resonances formalism in the description of processes involving Rydberg states of an excited atom, including features in the fluorescence spectrum partially caused by the quantum defect control due to ...

  11. An Attempt to automate the lithological classification of rocks using geological, gamma-spectrometric and satellite image datasets

    International Nuclear Information System (INIS)

    The present study aims essentially at proving that the application of the integrated airborne gamma spectrometric and satellite image data is capable of refining the mapped surface geology, and identification of anomalous zones of radioelement content that could provide favorable exploration targets for radioactive mineralizations.The application of the appropriate statistical technique to correlate between satellite image data and gamma-spectrometric data is of great significance in this respect. Experience shows that Landsat T M data in 7 spectral bands are successfully used in such studies rather than MSS. Multivariate statistical analysis techniques are applied to airborne spectrometric and different spectral Landsat T M data. Reduction of the data from n-dimensionality, both qualitatively as color composite image, and quantitatively, as principal component analysis, is performed using some statistical control parameters. This technique shows distinct efficiency in defining areas where different lit ho facies occur. An area located at the north of the Eastern Desert of Egypt, north of Hurgada town, was chosen to test the proposed technique of integrated interpretation of data of different physical nature. The reduced data are represented and interpreted both qualitatively and quantitatively. The advantages and limitations of applying such technique to the different airborne spectrometric, and Landsat T M data are identified. (authors)

  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. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

    OpenAIRE

    Hou, Xiaolin; Roos, Per

    2008-01-01

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for rad...

  14. 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...

  15. 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...

  16. Box-Behnken设计优化浊点萃取-原子荧光光谱法测定中药材中的汞%Cloud Point Extraction for Determination of Mercury in Chinese Herbal Medicine by Hydride Generation Atomic Fluorescence Spectrometry with Optimization Using Box-Behnken Design

    Institute of Scientific and Technical Information of China (English)

    王梅; 李姗; 周建栋; 徐英; 龙军标; 杨冰仪

    2014-01-01

    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 in-to 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·L-1 ,dithizone concentration of 4. 87 mol·L-1 ,and T 58. 2 ℃,the predicted value of fluorescence was 4 528. 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 1~5μg·L-1 .The limit of de-tection obtained was 0. 012 47 μg·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 tan-gerine samples with the recoveries of 95. 0%~100. 0%.Apparently Box- Behnken design combined with response surface anal-ysis method was

  17. THE ORNL ATOM PROBE

    OpenAIRE

    Miller, M

    1986-01-01

    The ORNL Atom Probe is a microanalytical tool for studies in materials science. The instrument is a combination of a customized version of the vacuum system of the VG FIM-100 atom probe, an ORNL-designed microcomputer-controlled digital timing system, and a double curved CEMA Imaging Atom Probe detector. The atom probe combines four instruments into one - namely a field ion microscope, an energy compensated time-of-flight mass spectrometer, an imaging atom probe, and a pulsed laser atom probe.

  18. 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

  19. 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)

  20. Ultraviolet fluorescence monitor

    Energy Technology Data Exchange (ETDEWEB)

    Hargis, P.J. Jr.; Preppernau, B.L.; Aragon, B.P. [Sandia National Labs., Albuquerque, NM (United States). Laser, Optics and Remote Sensing Dept.

    1997-05-01

    A multispectral ultraviolet (UV) fluorescence imaging fluorometer and a pulsed molecular beam laser fluorometer were developed to detect volatile organic compounds of interest in environmental monitoring and drug interdiction applications. The UV fluorescence imaging fluorometer is a relatively simple instrument which uses multiple excitation wavelengths to measure the excitation/emission matrix for irradiated samples. Detection limits in the high part-per-million to low part-per-million range were measured for a number of volatile organic vapors in the atmosphere. Detection limits in the low part-per-million range were obtained using cryogenic cooling to pre-concentrate unknown samples before introducing them into the imaging fluorometer. A multivariate analysis algorithm was developed to analyze the excitation/emission matrix and used to determine the relative concentrations of species in computer synthesized mixtures containing up to five organic compounds. Analysis results demonstrated the utility of multispectral UV fluorescence in analytical measurements. A transportable UV fluorescence imaging fluorometer was used in two field tests. Field test results demonstrated that detection limits in the part-per-billion range were needed to reliably identify volatile organic compounds in realistic field test measurements. The molecular beam laser fluorometer, a more complex instrument with detection limits in the part-per-billion to part-per-trillion range, was therefore developed to satisfy detection sensitivity requirements for field test measurements. High-resolution spectroscopic measurements made with the molecular beam laser fluorometer demonstrated its utility in identifying volatile organic compounds in the atmosphere.