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Sample records for absorption spectrometry measurements

  1. Ultraviolet and Light Absorption Spectrometry.

    ERIC Educational Resources Information Center

    Hargis, L. G.; Howell, J. A.

    1984-01-01

    Reviews developments in ultraviolet and light absorption spectrometry from December 1981 through November 1983, focusing on the chemistry involved in developing suitable reagents, absorbing systems, and methods of determination, and on physical aspects of the procedures. Includes lists of spectrophotometric methods for metals, non-metals, and…

  2. Algorithm development for intensity modulated continuous wave laser absorption spectrometry in atmospheric CO2 measurements

    NASA Astrophysics Data System (ADS)

    Lin, B.; Harrison, F. W.; Browell, E. V.; Dobler, J. T.; Bryant, R. B.

    2011-12-01

    Currently, NASA Langley Research Center (LaRC) and ITT are jointly developing algorithms for demonstration of range discrimination using ITT's laser absorption spectrometer (LAS), which is being evaluated for the future NASA Active Sensing of CO2 Emissions during Nights, Days, and Seasons (ASCENDS) mission. The objective of this Decadal Survey mission is to measure atmospheric column CO2 mixing ratios (XCO2) for improved determination of atmospheric carbon sources and sinks. Intensity Modulated Continuous Wave (IM-CW) techniques are used in this LAS approach. The LAS is designed to simultaneously measure CO2 and O2 columns, and these measurements are used to determine the required XCO2 column. The LAS measurements are enabled by the multi-channel operation of the instrument at 1.57 and 1.26-um for CO2 and O2, respectively. The algorithm development for the IM-CW techniques of the multi-channel LAS is focused on addressing key retrieval issues such as surface signal detection, thin cloud and/or aerosol layer rejection, vertical atmospheric range resolution, and optimizing the size of the measurement footprint. With these considerations, the modulation algorithm needs to maintain high enough signal-to-noise ratio (SNR) so that the mission scientific goals can be reached. A basic selection of the modulation algorithms that make XCO2 measurement and thin cloud rejection possible is the stepped frequency modulation scheme and a similar scheme of swept sine modulation. The differences between these two schemes for thin cloud rejection are small, assuming the proper selection of parameters is made. The stepped frequency approach is only a quantified version of swept sine method for the frequencies used. Swept sine scheme is a very common modulation technique for range discrimination, while the consideration of the stepped frequency scheme is based on the history of the rolling-tone modulation used in the instrument in previous successful column CO2 measurements. The

  3. Human Vitamin B12 Absorption and Metabolism are Measured by Accelerator Mass Spectrometry Using Specifically Labeled 14C-Cobalamin

    SciTech Connect

    Carkeet, C; Dueker, S R; Lango, J; Buchholz, B A; Miller, J W; Green, R; Hammock, B D; Roth, J R; Anderson, P J

    2006-01-26

    There is need for an improved test of human ability to assimilate dietary vitamin B{sub 12}. Assaying and understanding absorption and uptake of B{sub 12} is important because defects can lead to hematological and neurological complications. Accelerator mass spectrometry (AMS) is uniquely suited for assessing absorption and kinetics of {sup 14}C-labeled substances after oral ingestion because it is more sensitive than decay counting and can measure levels of carbon-14 ({sup 14}C) in microliter volumes of biological samples, with negligible exposure of subjects to radioactivity. The test we describe employs amounts of B{sub 12} in the range of normal dietary intake. The B{sub 12} used was quantitatively labeled with {sup 14}C at one particular atom of the DMB moiety by exploiting idiosyncrasies of Salmonellametabolism. In order to grow aerobically on ethanolamine, S. entericamust be provided with either pre-formed B{sub 12} or two of its precursors: cobinamide and dimethylbenzimidazole (DMB). When provided with {sup 14}C-DMB specifically labeled in the C2 position, cells produced {sup 14}C-B{sub 12} of high specific activity (2.1 GBq/mmol, 58 mCi/mmol) and no detectable dilution of label from endogenous DMB synthesis. In a human kinetic study, a physiological dose (1.5 mg, 2.2 KBq/59 nCi) of purified {sup 14}C-B{sub 12} was administered and showed plasma appearance and clearance curves consistent with the predicted behavior of the pure vitamin. This method opens new avenues for study of B{sub 12} assimilation.

  4. Determination of inorganic and total mercury by vapor generation atomic absorption spectrometry using different temperatures of the measurement cell

    NASA Astrophysics Data System (ADS)

    Kaercher, Luiz Eduardo; Goldschmidt, Fabiane; Paniz, José Neri Gottfried; de Moraes Flores, Érico Marlon; Dressler, Valderi Luiz

    2005-06-01

    A simple and inexpensive laboratory-built flow injection vapor generation system coupled to atomic absorption spectrometry (FI-VG AAS) for inorganic and total mercury determination has been developed. It is based on the vapor generation of total mercury and a selective detection of Hg 2 + or total mercury by varying the temperature of the measurement cell. Only the inorganic mercury is measured when the quartz cell is at room temperature, and when the cell is heated to 650 °C or higher the total Hg concentration is measured. The organic Hg concentration in the sample is calculated from the difference between the total Hg and Hg 2 + concentrations. Parameters such as the type of acid (HCl or HNO 3) and its concentration, reductant (NaBH 4) concentration, carrier solution (HCl) flow rate, carrier gas flow rate, sample volume and quartz cell temperature, which influence FI-VG AAS system performance, were systematically investigated. The optimized conditions for Hg 2 + and total Hg determinations were: 1.0 mol l - 1 HCl as carrier solution, carrier flow rate of 3.5 ml min - 1 , 0.1% (m/v) NaBH 4, reductant flow rate of 1.0 ml min - 1 and carrier gas flow rate of 200 ml min - 1 . The relative standard deviation (RSD) is lower than 5.0% for a 1.0 μg l - 1 Hg solution and the limit of quantification (LOQ, 10 s) is 55 ng g - 1 . Certified samples of dogfish muscle (DORM-1 and DORM-2) and non-certified fish samples were analyzed, using a 6.0 mol l - 1 HCl solution for analyte extraction. The Hg 2 + and CH 3Hg + concentrations found were in agreement with certified ones.

  5. Atomic Absorption, Atomic Fluorescence, and Flame Emission Spectrometry.

    ERIC Educational Resources Information Center

    Horlick, Gary

    1984-01-01

    This review is presented in six sections. Sections focus on literature related to: (1) developments in instrumentation, measurement techniques, and procedures; (2) performance studies of flames and electrothermal atomizers; (3) applications of atomic absorption spectrometry; (4) analytical comparisons; (5) atomic fluorescence spectrometry; and (6)…

  6. 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

    ERIC Educational Resources Information Center

    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,…

  7. Absorption mode FTICR mass spectrometry imaging.

    PubMed

    Smith, Donald F; Kilgour, David P A; Konijnenburg, Marco; O'Connor, Peter B; Heeren, Ron M A

    2013-12-03

    Fourier transform ion cyclotron resonance mass spectrometry offers the highest mass resolving power for molecular imaging experiments. This high mass resolving power ensures that closely spaced peaks at the same nominal mass are resolved for proper image generation. Typically higher magnetic fields are used to increase mass resolving power. However, a gain in mass resolving power can also be realized by phase correction of the data for absorption mode display. In addition to mass resolving power, absorption mode offers higher mass accuracy and signal-to-noise ratio over the conventional magnitude mode. Here, we present the first use of absorption mode for Fourier transform ion cyclotron resonance mass spectrometry imaging. The Autophaser algorithm is used to phase correct each spectrum (pixel) in the image, and then, these parameters are used by the Chameleon work-flow based data processing software to generate absorption mode "Datacubes" for image and spectral viewing. Absorption mode reveals new mass and spatial features that are not resolved in magnitude mode and results in improved selected ion image contrast.

  8. Optical absorption measurement system

    DOEpatents

    Draggoo, Vaughn G.; Morton, Richard G.; Sawicki, Richard H.; Bissinger, Horst D.

    1989-01-01

    The system of the present invention contemplates a non-intrusive method for measuring the temperature rise of optical elements under high laser power optical loading to determine the absorption coefficient. The method comprises irradiating the optical element with a high average power laser beam, viewing the optical element with an infrared camera to determine the temperature across the optical element and calculating the absorption of the optical element from the temperature.

  9. Graphite filter atomizer in atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Katskov, Dmitri A.

    2007-09-01

    Graphite filter atomizers (GFA) for electrothermal atomic absorption spectrometry (ETAAS) show substantial advantages over commonly employed electrothermal vaporizers and atomizers, tube and platform furnaces, for direct determination of high and medium volatility elements in matrices associated with strong spectral and chemical interferences. Two factors provide lower limits of detection and shorter determination cycles with the GFA: the vaporization area in the GFA is separated from the absorption volume by a porous graphite partition; the sample is distributed over a large surface of a collector in the vaporization area. These factors convert the GFA into an efficient chemical reactor. The research concerning the GFA concept, technique and analytical methodology, carried out mainly in the author's laboratory in Russia and South Africa, is reviewed. Examples of analytical applications of the GFA in AAS for analysis of organic liquids and slurries, bio-samples and food products are given. Future prospects for the GFA are discussed in connection with analyses by fast multi-element AAS.

  10. Validation and application of cavity-enhanced, near-infrared tunable diode laser absorption spectrometry for measurements of methane carbon isotopes at ambient concentrations.

    PubMed

    Mortazavi, Behzad; Wilson, Benjamin J; Dong, Feng; Gupta, Manish; Baer, Doug

    2013-10-15

    Methane is an effective greenhouse gas but has a short residence time in the atmosphere, and therefore, reductions in emissions can alleviate its greenhouse gas warming effect within a decadal time frame. Continuous and high temporal resolution measurements of methane concentrations and carbon isotopic ratios (δ(13)CH4) can inform on mechanisms of formation, provide constraints on emissions sources, and guide future mitigation efforts. We describe the development, validation, and deployment of a cavity-enhanced, near-infrared tunable diode laser absorption spectrometry system capable of quantifying δ(13)CH4 at ambient methane concentrations. Laboratory validation and testing show that the instrument is capable of operating over a wide dynamic range of methane concentration and provides a measurement precision for δ(13)CH4 of better than ± 0.5 ‰ (1σ) over 1000 s of data averaging at ambient methane concentrations. The analyzer is accurate to better than ± 0.5 ‰, as demonstrated by measurements of characterized methane/air samples with minimal dependence (<1 ‰) of measured carbon isotope ratio on methane concentration. Deployment of the instrument at a marsh over multiple days demonstrated how methane fluxes varied by an order of magnitude over 2 day deployment periods, and showed a 17 ‰ variability in δ(13)CH4 of the emitted methane during the growing season.

  11. Lead and cadmium in human placentas and maternal and neonatal blood (in a heavily polluted area) measured by graphite furnace atomic absorption spectrometry.

    PubMed Central

    Baranowska, I

    1995-01-01

    OBJECTIVE--To measure the concentrations of the trace elements lead and cadmium in human placenta and in maternal and neonatal (cord) blood. To assess the influence of the strongly polluted environment on the content of metals in tissues and on the permeability of placenta to cadmium and lead. Various methods of mineralisation were tested before analysis. METHODS--Graphite furnace atomic absorption spectrometry was used for the determination of lead and cadmium. The samples for analysis were prepared by mineralisation under pressure in a Teflon bomb (HNO3, 110 degrees C), by wet ashing under normal pressure (HNO3 + H2O2 for 12 hours), and by microwave digestion in concentrated nitric acid. RESULTS--In analysed samples the following mean concentrations of cadmium and lead were found: in venous blood Pb = 72.50 ng/ml, Cd = 4.90 ng/ml; in placenta Pb = 0.50 microgram/g, Cd = 0.11 microgram/g; in cord blood Pb = 38.31 ng/ml, Cd = 1.13 ng/ml. CONCLUSION--High concentrations of lead and cadmium were found in placentas and in maternal blood whereas in neonatal blood there was an increased concentration of lead and only traces of cadmium. It is concluded that the placenta is a better barrier for cadmium than for lead. Among the examined methods of mineralisation, microwave digestion was the best. PMID:7795737

  12. DETERMINATION OF TOTAL MERCURY IN FISH TISSUES USING PYROLYSIS ATOMIC ABSORPTION SPECTROMETRY WITH GOLD AMALGAMATION

    EPA Science Inventory

    A simple and rapid procedure for measuring total mercury in fish tissues is evaluated and
    compared with conventional techniques. Using an automated instrument incorporating combustion, preconcentration by amalgamation with gold, and atomic absorption spectrometry (AAS), mill...

  13. Absorption Mode FT-ICR Mass Spectrometry Imaging

    SciTech Connect

    Smith, Donald F.; Kilgour, David P.; Konijnenburg, Marco; O'Connor, Peter B.; Heeren, Ronald M.

    2013-12-03

    Fourier transform ion cyclotron resonance mass spectrometry offers the highest mass resolving power for molecular imaging experiments. This high mass resolving power ensures that closely spaced peaks at the same nominal mass are resolved for proper image generation. Typically higher magnetic fields are used to increase mass resolving power. However, a gain in mass resolving power can also be realized by phase correction of the data for absorption mode display. In addition to mass resolving power, absorption mode offers higher mass accuracy and signal-to-noise ratio over the conventional magnitude mode. Here we present the first use of absorption mode for Fourier transform ion cyclotron resonance mass spectrometry imaging. The Autophaser algorithm is used to phase correct each spectrum (pixel) in the image and then these parameters are used by the Chameleon work-flow based data processing software to generate absorption mode ?Datacubes? for image and spectral viewing. Absorption mode reveals new mass and spatial features that are not resolved in magnitude mode and results in improved selected ion image contrast.

  14. [Application of atomic absorption spectrometry in the engine knock detection].

    PubMed

    Chen, Li-Dan

    2013-02-01

    Because existing human experience diagnosis method and apparatus for auxiliary diagnosis method are difficult to diagnose quickly engine knock. Atomic absorption spectrometry was used to detect the automobile engine knock in in innovative way. After having determined Fe, Al, Cu, Cr and Pb content in the 35 groups of Audi A6 engine oil whose travel course is 2 000 -70 000 kilometers and whose sampling interval is 2 000 kilometers by atomic absorption spectrometry, the database of primary metal content in the same automobile engine at different mileage was established. The research shows that the main metal content fluctuates within a certain range. In practical engineering applications, after the determination of engine oil main metal content and comparison with its database value, it can not only help to diagnose the type and location of engine knock without the disintegration and reduce vehicle maintenance costs and improve the accuracy of engine knock fault diagnosis.

  15. Aerosol Absorption Measurements in MILAGRO.

    NASA Astrophysics Data System (ADS)

    Gaffney, J. S.; Marley, N. A.; Arnott, W. P.; Paredes-Miranda, L.; Barnard, J. C.

    2007-12-01

    During the month of March 2006, a number of instruments were used to determine the absorption characteristics of aerosols found in the Mexico City Megacity and nearby Valley of Mexico. These measurements were taken as part of the Department of Energy's Megacity Aerosol Experiment - Mexico City (MAX-Mex) that was carried out in collaboration with the Megacity Interactions: Local and Global Research Observations (MILAGRO) campaign. MILAGRO was a joint effort between the DOE, NSF, NASA, and Mexican agencies aimed at understanding the impacts of a megacity on the urban and regional scale. A super-site was operated at the Instituto Mexicano de Petroleo in Mexico City (designated T-0) and at the Universidad Technologica de Tecamac (designated T-1) that was located about 35 km to the north east of the T-0 site in the State of Mexico. A third site was located at a private rancho in the State of Hidalgo approximately another 35 km to the northeast (designated T-2). Aerosol absorption measurements were taken in real time using a number of instruments at the T-0 and T-1 sites. These included a seven wavelength aethalometer, a multi-angle absorption photometer (MAAP), and a photo-acoustic spectrometer. Aerosol absorption was also derived from spectral radiometers including a multi-filter rotating band spectral radiometer (MFRSR). The results clearly indicate that there is significant aerosol absorption by the aerosols in the Mexico City megacity region. The absorption can lead to single scattering albedo reduction leading to values below 0.5 under some circumstances. The absorption is also found to deviate from that expected for a "well-behaved" soot anticipated from diesel engine emissions, i.e. from a simple 1/lambda wavelength dependence for absorption. Indeed, enhanced absorption is seen in the region of 300-450 nm in many cases, particularly in the afternoon periods indicating that secondary organic aerosols are contributing to the aerosol absorption. This is likely due

  16. The role of atomic absorption spectrometry in geochemical exploration

    USGS Publications Warehouse

    Viets, J.G.; O'Leary, R. M.

    1992-01-01

    In this paper we briefly describe the principles of atomic absorption spectrometry (AAS) and the basic hardware components necessary to make measurements of analyte concentrations. Then we discuss a variety of methods that have been developed for the introduction of analyte atoms into the light path of the spectrophotometer. This section deals with sample digestion, elimination of interferences, and optimum production of ground-state atoms, all critical considerations when choosing an AAS method. Other critical considerations are cost, speed, simplicity, precision, and applicability of the method to the wide range of materials sampled in geochemical exploration. We cannot attempt to review all of the AAS methods developed for geological materials but instead will restrict our discussion to some of those appropriate for geochemical exploration. Our background and familiarity are reflected in the methods we discuss, and we have no doubt overlooked many good methods. Our discussion should therefore be considered a starting point in finding the right method for the problem, rather than the end of the search. Finally, we discuss the future of AAS relative to other instrumental techniques and the promising new directions for AAS in geochemical exploration. ?? 1992.

  17. [Measurement and analysis of absorption spectrum of human blood].

    PubMed

    Zhao, Zhi-Min; Xin, Yu-Jun; Wang, Le-Xin; Zhu, Wei-Hua; Zheng, Min; Guo, Xin

    2008-01-01

    The present paper puts forward a method of disease diagnosis by using the technology of spectrum analysis of human blood serum. The generation mechanism of absorption spectrum is explained and the absorption spectra of the normal blood serum and the sick blood serum are listed from the experiments of absorption spectrometry. Though the value of absorbency of the sick blood serum is almost equal to that of the normal blood serum in the most absorption spectra, there are some differences around 278 nm in the absorption spectrum. The absorbency of the blood serum with hyperglycemia is greater than that of the normal blood serum at 285 nm in the spectrum, and besides, there comes a peak shift of absorption with hyperglycemia. In the absorption spectrum of the blood serum with hypercholesterolemia, there is a clear absorption peak at 414 nm. However there is not any peak at that wavelength in the absorption spectrum of the normal blood serum. Through comparing the characters of the spectrum, we can judge if the blood sample is or not, and this blood analysis is a new method for the diagnosis of disease. Compared with other methods of blood measurements, the method of absorption spectrum analysis of blood serum presented in this paper, is more convenient for measurement, simpler for analysis, and easier to popularize.

  18. Metal content monitoring in Hypericum perforatum pharmaceutical derivatives by atomic absorption and emission spectrometry.

    PubMed

    Gomez, María R; Soledad, Cerutti; Olsina, Roberto A; Silva, María F; Martínez, Luis D

    2004-02-18

    Metals have been investigated in different plant materials in order to establish their normal concentration range and consider their role in plants as part of human medicinal treatment. Metal monitoring as a pattern recognition method is a promising tool in the characterization and/or standardization of phytomedicines. In the present work measurable amounts of Ca, Cu, K, Li, Mg, Mn, Na, Ni, and Zn were detected in phytopharmaceutical derivatives of Hypericum perforatum by atomic techniques. Atomic methodologies like flame atomic absorption spectrometry (FAAS) and electrothermal atomic absorption spectrometry (ETAAS) allow reliable determination of mineral content in pharmaceutical quality control of medicinal plants. Additionally, capillary electrophoresis (CE) patterns of characteristic components (fingerprints) have been performed for the search of adulterants in phytopharmaceutical products.

  19. Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater: A Laboratory Exercise

    ERIC Educational Resources Information Center

    Correia, Paulo R. M.; Oliveira, Pedro V.

    2004-01-01

    The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

  20. Determination of mercury in hair: Comparison between gold amalgamation-atomic absorption spectrometry and mass spectrometry.

    PubMed

    Domanico, Francesco; Forte, Giovanni; Majorani, Costanza; Senofonte, Oreste; Petrucci, Francesco; Pezzi, Vincenzo; Alimonti, Alessandro

    2016-09-29

    Mercury is a heavy metal that causes serious health problems in exposed subjects. The most toxic form, i.e., methylmercury (MeHg), is mostly excreted through human hair. Numerous analytical methods are available for total Hg analysis in human hair, including cold vapour atomic fluorescence spectrometry (CV-AFS), inductively coupled plasma mass spectrometry (ICP-MS) and thermal decomposition amalgamation atomic absorption spectrometry (TDA-AAS). The aim of the study was to compare the TDA-AAS with the ICP-MS in the Hg quantification in human hair. After the washing procedure to minimize the external contamination, from each hair sample two aliquots were taken; the first was used for direct analysis of Hg by TDA-AAS and the second was digested for Hg determination by the ICP-MS. Results indicated that the two data sets were fully comparable (median; TDA-AAS, 475ngg(-1); ICP-MS, 437ngg(-1)) and were not statistically different (Mann-Whitney test; p=0.44). The two techniques presented results with a good coefficient of correlation (r=0.94) despite different operative ranges and method limits. Both techniques satisfied internal performance requirements and the parameters for method validation resulting sensitive, precise and reliable. Finally, the use of the TDA-AAS can be considered instead of the ICP-MS in hair analysis in order to reduce sample manipulation with minor risk of contamination, less time consuming due to the absence of the digestion step and cheaper analyses.

  1. Investigation of chemical modifiers for phosphorus in a graphite furnace using high-resolution continuum source atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Lepri, Fábio G.; Dessuy, Morgana B.; Vale, Maria Goreti R.; Borges, Daniel L. G.; Welz, Bernhard; Heitmann, Uwe

    2006-08-01

    Phosphorus is not one of the elements that are typically determined by atomic absorption spectrometry, but this technique nevertheless offers several advantages that make it attractive, such as the relatively great freedom from interferences. As the main resonance lines for phosphorus are in the vacuum-ultraviolet, inaccessible by conventional atomic absorption spectrometry equipment, Ĺvov and Khartsyzov proposed to use the non-resonance doublet at 213.5 / 213.6 nm. Later it turned out that with conventional equipment it is necessary to use a chemical modifier in order to get reasonable sensitivity, and lanthanum was the first one suggested for that purpose. In the following years more than 30 modifiers have been proposed for the determination of this element, and there is no consensus about the best one. In this work high-resolution continuum source atomic absorption spectrometry has been used to investigate the determination of phosphorus without a modifier and with the addition of selected modifiers of very different nature, including the originally recommended lanthanum modifier, several palladium-based modifiers and sodium fluoride. As high-resolution continuum source atomic absorption spectrometry is revealing the spectral environment of the analytical line at high resolution, it became obvious that without the addition of a modifier essentially no atomic phosphorus is formed, even at 2700 °C. The absorption measured with line source atomic absorption spectrometry in this case is due to the PO molecule, the spectrum of which is overlapping with the atomic line. Palladium, with or without the addition of calcium or ascorbic acid, was found to be the only modifier to produce almost exclusively atomic phosphorus. Lanthanum and particularly sodium fluoride produced a mixture of P and PO, depending on the atomization temperature. This fact can explain at least some of the discrepancies found in the literature and some of the phenomena observed in the

  2. Determination of nanogram amounts of bismuth in rocks by atomic absorption spectrometry with electrothermal atomization

    USGS Publications Warehouse

    Kane, J.S.

    1979-01-01

    Bismuth concentrations as low as 10 ng g-1 in 100-mg samples of geological materials can be determined by atomic absorption spectrometry with electrothermal atomization. After HF-HClO4 decomposition of the sample, bismuth is extracted as the iodide into methyl isobutyl ketone and is then stripped with ethylenediaminetetraacetic acid into the aqueous phase. Aliquots of this solution are pipetted into the graphite furnace and dried, charred, and atomized in an automated sequence. Atomic absorbance at the Bi 223.1-nm line provides a measure of the amount of bismuth present. Results are presented for 14 U.S. Geological Survey standard rocks. ?? 1979.

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

    PubMed

    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.

  4. Determination of tetraalkyllead compounds in gasoline by liquid chromatography-atomic absorption spectrometry

    USGS Publications Warehouse

    Messman, J.D.; Rains, T.C.

    1981-01-01

    A liquid chromatography-atomic absorption spectrometry (LC-AAS) hybrid analytical technique is presented for metal speciation measurements on complex liquid samples. The versatility and inherent metal selectivity of the technique are Illustrated by the rapid determination of five tetraalkyllead compounds in commercial gasoline. Separation of the individual tetraalkyllead species is achieved by reversed-phase liquid chromatography using an acetonitrile/water mobile phase. The effluent from the liquid Chromatograph Is introduced directly into the aspiration uptake capillary of the nebulizer of an air/acetylene flame atomic absorption spectrometer. Spectral interferences due to coeluting hydrocarbon matrix constituents were not observed at the 283.3-nm resonance line of lead used for analysis. Detection limits of this LC-AAS hydrid analytical technique, based on a 20-??L injection, are approximately 10 ng Pb for each tetraalkyllead compound.

  5. EPA Method 245.1: Determination of Mercury in Water by Cold Vapor Atomic Absorption Spectrometry

    EPA Pesticide Factsheets

    SAM lists this method for preparation and analysis of aqueous liquid and drinking water samples. This method will determine mercuric chloride and methoxyethylmercuric acetate as total mercury using cold vapor atomic absorption spectrometry.

  6. Determination of Hg, Cd, Mn, Pb and Sn in seafood by solid sampling Zeeman atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Detcheva, A.; Grobecker, K. H.

    2006-04-01

    Direct solid sampling Zeeman atomic absorption spectrometric methods were developed and applied to the determination of mercury, cadmium, manganese, lead and tin in seafood. All elements but mercury were measured by a third generation Zeeman atomic absorption spectrometry combined with an automatic solid sampler. In 3-field- and dynamic mode the calibrations concentration range was substantially extended and high amounts of analyte were detectable without laborious dilution of solid samples. The measurements were based on calibrations using certified reference materials of organic matrices. In case solid certified reference materials were not available calibration by aqueous standard solutions was proved to be an alternative. No matrix effects were observed under the optimized conditions. Results obtained were in good agreement with the certified values. Solid sampling Zeeman atomic absorption spectrometry proved to be a reliable, rapid and low-cost method for the control of trace elements in seafood.

  7. High temperature measurement of water vapor absorption

    NASA Technical Reports Server (NTRS)

    Keefer, Dennis; Lewis, J. W. L.; Eskridge, Richard

    1985-01-01

    An investigation was undertaken to measure the absorption coefficient, at a wavelength of 10.6 microns, for mixtures of water vapor and a diluent gas at high temperature and pressure. The experimental concept was to create the desired conditions of temperature and pressure in a laser absorption wave, similar to that which would be created in a laser propulsion system. A simplified numerical model was developed to predict the characteristics of the absorption wave and to estimate the laser intensity threshold for initiation. A non-intrusive method for temperature measurement utilizing optical laser-beam deflection (OLD) and optical spark breakdown produced by an excimer laser, was thoroughly investigated and found suitable for the non-equilibrium conditions expected in the wave. Experiments were performed to verify the temperature measurement technique, to screen possible materials for surface initiation of the laser absorption wave and to attempt to initiate an absorption wave using the 1.5 kW carbon dioxide laser. The OLD technique was proven for air and for argon, but spark breakdown could not be produced in helium. It was not possible to initiate a laser absorption wave in mixtures of water and helium or water and argon using the 1.5 kW laser, a result which was consistent with the model prediction.

  8. Microdroplet Sample Application in Electrothermal Atomization for Atomic Absorption Spectrometry.

    DTIC Science & Technology

    1982-03-29

    ad ideftify by Week amber) atomic absorption spectroscopy microsampl ing graphite- furnace AAS automation C> 20. AOSTRACT (Coninuhe an reveresi de It...furnace and spectrometer system as well as for partial support of this project. REFERENCES 1. J. D. Winefordner, Atomic Absorption Spectroscopy , G. F

  9. Differentiation and classification of beers with flame atomic spectrometry and molecular absorption spectrometry and sample preparation assisted by microwaves

    NASA Astrophysics Data System (ADS)

    Bellido-Milla, Dolores; Moreno-Perez, Juana M.; Hernández-Artiga, María. P.

    2000-07-01

    The characterization of beer samples has a lot of interest because their composition can affect the taste and stability of beer and consumer health. Flame atomic absorption spectrometry was used to determine Fe, Mn, Zn, Cu, Mg, Ca and Al. Sodium and K were determined by flame atomic emission spectrometry. A sample preparation method was developed, based on treatment with HNO 3 and H 2O 2 in a microwave oven. This has many advantages over the methods found in the literature. The combination of the results of atomic spectrometry and the spectrum obtained by molecular absorption spectrometry provides information on the inorganic and organic components of the samples. The application of chemometric techniques to chemical composition data could be extremely useful for food quality control. The metal concentrations, the molecular absorption spectrum, the pH and conductivity of each sample were subject to analysis of variance and linear discriminant analysis. Twenty-five different beer samples were used to differentiate and classify different types of beers.

  10. Room-temperature study of iron gall ink impregnated paper degradation under various oxygen and humidity conditions: time-dependent monitoring by viscosity and X-ray absorption near-edge spectrometry measurements.

    PubMed

    Rouchon, Véronique; Duranton, Maroussia; Burgaud, Cédric; Pellizzi, Eleonora; Lavédrine, Bertrand; Janssens, Koen; de Nolf, Wout; Nuyts, Gert; Vanmeert, Frederik; Hellemans, Kevin

    2011-04-01

    Many western manuscripts were written using iron gall inks. These inks can damage the paper via two major mechanisms: (a) acid hydrolysis, enhanced by humidity, and (b) oxidative depolymerization provoked by the presence of oxygen and free iron(II) ions. The degradation of unsized Whatman paper impregnated with different combinations of iron sulfate, gallic acid, and gum arabic was studied at room temperature in order to assess the relative importance of each mechanism. The samples were stored in various environments including a dry and/or an oxygen-free atmosphere. The cellulose depolymerization was monitored by viscometry and related to changes in the oxidation state of iron, determined by X-ray absorption near-edge spectrometry. The results indicate that residual amounts of oxygen (less than 0.1%) promote cellulose depolymerization, whereas the level of relative humidity has no impact. The cellulose depolymerization also appears closely correlated to oxidative mechanisms. Regarding the oxidation of iron, it only occurs in the simultaneous presence of oxygen and moisture, suggesting the occurrence of rustlike oxidative mechanisms. Finally, the presence of gallic acid has a strong influence, which is only partially explained by its capacity to reduce iron(III) to iron(II).

  11. OH measurement by laser light absorption

    NASA Technical Reports Server (NTRS)

    Perner, D.

    1986-01-01

    Since the first attempt to measure atmospheric hydroxyl radicals by optical absorption in 1975 (Perner et al., 1976) this method has been continuously developed further and its major obstacles and limitations are known today. The laser beam needs to be expanded in order to reduce the beam divergence. At the same time the energy density of the laser beam which produces OH via ozone photolysis is reduced to such an extent that the self-produced OH concentration ranges well below the atmospheric value. Atmospheric absorptions should be observed over a wide spectral range so that not only the OH radicals are properly identified by several rotational lines but their absorption can be corrected for interfering absorptions from other air constituents as SO2, CH2O, CS2, etc., which can be identified in a wide spectral range with more confidence. Air turbulence demands fast spectral scanning or probing on and off the absorption line. Energy requirements should be kept small in field operations. In the experiment frequency doubled dye laser pulses at 308 nm are produced. The picosecond light pulses are expected to show a smooth profile (light intensity against wavelength) which will be broadened to the required spectral width according to the uncertainty principle. The pump laser will be an optoacoustically modulated Nd:YAG laser.

  12. Study of the analytical methods for iron determination in complex organic liquids by atomic absorption spectrometry

    SciTech Connect

    Torre, M.; Gonzalez, M.C.; Jimenez, O.; Rodriquez, A.R. )

    1990-01-01

    In the determination of iron in complex organic liquids by atomic absorption spectrometry (A.A.S.), methods of sample preparation, such as dilution with an organic solvent and sample pretreatment to destroy organic material, are investigated. Moreover, methods of analysis using calibration curve and standard additions are presented. The possible cause of error associated with iron determination in organic samples by flame (F-A.A.S.) and graphite furnace (GF-A.A.S.) atomic absorption spectrometry are discussed. From all of these studies, the use of graphite furnace atomic absorption spectrometry after sample dilution with methyl isobutyl ketone, and the use of the method of standard additions are advised for iron determination.

  13. The direct determination of HgS by thermal desorption coupled with atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Coufalík, Pavel; Zvěřina, Ondřej; Komárek, Josef

    2016-04-01

    This research was aimed at the direct determination of HgS in environmental samples by means of thermal desorption coupled with atomic absorption spectrometry. Operating parameters of the apparatus used for thermal desorption (including a prototype desorption unit) are described in this work, as well as the procedure for measuring mercury release curves together with an evaluation of the analytical signal including two methods of peak integration. The results of thermal desorption were compared with HgS contents obtained by sequential extraction. The limits of quantification of the proposed method for the selective determination of the black and red forms of HgS were 4 μg kg- 1 and 5 μg kg- 1, respectively. The limit of quantification of red HgS in soils was 35 μg kg- 1. The developed analytical procedure was applied to soil and sediment samples from historical mining areas.

  14. Slurry sampling electrothermal atomic absorption spectrometry as screening method for chromium in compost.

    PubMed

    Laborda, F; Górriz, M P; Castillo, J R

    2004-10-20

    Ultrasonic slurry sample introduction was applied to the determination of total chromium in composted materials by electrothermal atomic absorption spectrometry (ETAAS). The effect of grinding on the heterogeneity of the test samples and on the attainable precision was studied. The repeatability was influenced by the heterogeneity of the test samples at the mug-level, the R.S.D. of the measurements being 15%. The reproducibility depended on the heterogeneity of the test sample at the mg level, and it could be improved from 11 to 7% by increasing the grinding time. The characteristic mass was 2.6pg and the detection limit for the optimised procedure at the 0.04% (w/v) slurry concentration, 370ngg(-1). Good agreement with a certified reference material and with the conventional microwave assisted digestion method was found by using external calibration with aqueous standards. The performance of the method for screening purposes was evaluated.

  15. Piezoelectric-tuned microwave cavity for absorption spectrometry

    DOEpatents

    Leskovar, Branko; Buscher, Harold T.; Kolbe, William F.

    1978-01-01

    Gas samples are analyzed for pollutants in a microwave cavity that is provided with two highly polished walls. One wall of the cavity is mechanically driven with a piezoelectric transducer at a low frequency to tune the cavity over a band of microwave frequencies in synchronism with frequency modulated microwave energy applied to the cavity. Absorption of microwave energy over the tuned frequencies is detected, and energy absorption at a particular microwave frequency is an indication of a particular pollutant in the gas sample.

  16. Resonance ionization mass spectrometry for isotopic abundance measurements

    NASA Technical Reports Server (NTRS)

    Miller, C. M.

    1986-01-01

    Resonance ionization mass spectrometry (RIMS) is a relatively new laser-based technique for the determination of isotopic abundances. The resonance ionization process depends upon the stepwise absorption of photons from the laser, promoting atoms of the element of interest through progressively higher electronic states until an ion is formed. Sensitivity arises from the efficiency of the resonant absorption process when coupled with the power available from commercial laser sources. Selectivity derives naturally from the distinct electronic structure of different elements. This isobaric discrimination has provided the major impetus for development of the technique. Resonance ionization mass spectrometry was used for analysis of the isotopic abundances of the rare earth lutetium. Isobaric interferences from ytterbium severely effect the ability to measure small amounts of the neutron-deficient Lu isotopes by conventional mass spectrometric techniques. Resonance ionization for lutetium is performed using a continuous-wave laser operating at 452 nm, through a sequential two-photon process, with one photon exciting the intermediate resonance and the second photon causing ionization. Ion yields for microgram-sized quantities of lutetium lie between 10(6) and 10(7) ions per second, at overall ionization efficiencies approaching 10(-4). Discrimination factors against ytterbium greater than 10(6) have been measured. Resonance ionization for technetium is also being explored, again in response to an isobaric interference, molybdenum. Because of the relatively high ionization potential for Tc, three-photon, two-color RIMS processes are being developed.

  17. Selection of the optimal combination of water vapor absorption lines for detection of temperature in combustion zones of mixing supersonic gas flows by diode laser absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mironenko, V. R.; Kuritsyn, Yu. A.; Bolshov, M. A.; Liger, V. V.

    2016-12-01

    Determination of a gas medium temperature by diode laser absorption spectrometry (DLAS) is based on the measurement of integral intensities of the absorption lines of a test molecule (generally water vapor molecule). In case of local thermodynamic equilibrium temperature is inferred from the ratio of the integral intensities of two lines with different low energy levels. For the total gas pressure above 1 atm the absorption lines are broadened and one cannot find isolated well resolved water vapor absorption lines within relatively narrow spectral interval of fast diode laser (DL) tuning range (about 3 cm-1). For diagnostics of a gas object in the case of high temperature and pressure DLAS technique can be realized with two diode lasers working in different spectral regions with strong absorption lines. In such situation the criteria of the optimal line selection differs significantly from the case of narrow lines. These criteria are discussed in our work. The software for selection the optimal spectral regions using the HITRAN-2012 and HITEMP data bases is developed. The program selects spectral regions of DL tuning, minimizing the error of temperature determination δT/T, basing on the attainable experimental error of line intensity measurement δS. Two combinations of optimal spectral regions were selected - (1.392 & 1.343 μm) and (1.392 & 1.339 μm). Different algorithms of experimental data processing are discussed.

  18. High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

    2017-03-01

    In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

  19. Ultrafast transient absorption measurements of heme proteins

    NASA Astrophysics Data System (ADS)

    Ye, Xiong; Demidov, Andrey; Wang, Wei; Christian, James; Champion, Paul

    1998-03-01

    Transient absorption spectra reveal the dynamics and intermediate states of the heme active site after ligand photodissociation, which helps clarify the physical process of ligand dissociation and geminate recombination. To measure the transient absorption spectra, we apply a femtosecond pump-probe technique with frequency resolved detection using a multichannel diode array. The femtosecond pulse output from a regenerative laser amplifier system is split in two; one beam pumps the optical parametric amplifier to produce a tunable wavelength pump pulse, the other beam generates a white light continuum that is varied in time with respect to pump pulse and probe the transient absorbance of the sample. We make a comparative study of myoglobin with different ligands, mutants and pH conditions.

  20. Determination of arsenic and selenium in environmental and agricultural samples by hydride generation atomic absorption spectrometry

    SciTech Connect

    Hershey, J.W.; Oostdyk, T.S.; Keliher, P.N.

    1988-11-01

    Agricultural and environmental samples are digested with acid, and arsenic and selenium are determined using hydride generation atomic absorption spectrometry. Interelement interferences are eliminated by high acid concentrations or cation-exchange resins. Agreement with standard reference material is excellent. The technique is also applied to actual samples.

  1. COMPREHENSIVE ANALYSIS OF BIOLOGICALLY RELEVANT ARSENICALS BY PH-SELECTIVE HYDRIDE GENERATION-ATOMIC ABSORPTION SPECTROMETRY

    EPA Science Inventory


    A method based on pH-selective generation and separation of arsines is commonly used for analysis of inorganic, methylated, and dimethylated trivalent and pentavalent arsenicals by hydride generation-atomic absorption spectrometry (HG-AAS). We have optimized this method to pe...

  2. Modeling optical absorption for thermoreflectance measurements

    NASA Astrophysics Data System (ADS)

    Yang, Jia; Ziade, Elbara; Schmidt, Aaron J.

    2016-03-01

    Optical pump-probe techniques based on thermoreflectance, such as time domain thermoreflectance and frequency domain thermoreflectance (FDTR), have been widely used to characterize the thermal conductivity of thin films and the thermal conductance across interfaces. These techniques typically use a transducer layer to absorb the pump light and improve the thermoreflectance signal. The transducer, however, complicates the interpretation of the measured signal because the approximation that all the energy from the pump beam is deposited at the transducer surface is not always accurate. In this paper, we consider the effect of laser absorption in the top layer of a multilayer sample, and derive an analytical solution for the thermoreflectance signal in the diffusion regime based on volumetric heating. We analyze the measurement sensitivity to the pump absorption depth for transducers with different thermal conductivities, and investigate the additional effect of probe laser penetration depth on the measured signal. We validate our model using FDTR measurements on 490 nm thick amorphous silicon films deposited on fused silica and silicon substrates.

  3. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L- 1 HNO3 solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L- 1 and 36.4 mg L- 1, respectively. The repeatability of the results expressed as relative standard deviation was typically < 5%. The accuracy of the method was tested by analysis of digested biological certified reference materials (soya bean flour, corn flour and herbs) and recovery experiment for beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93-105% with the repeatability in the range of 4.1-5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg- 1), egg white (2188 ± 29 mg kg- 1), mineral water (31.0 ± 0.9 mg L- 1), white wine (260 ± 4 mg L- 1) and red wine (82 ± 2 mg L- 1), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L- 1).

  4. Near edge X-ray absorption mass spectrometry on coronene

    SciTech Connect

    Reitsma, G.; Deuzeman, M. J.; Hoekstra, R.; Schlathölter, T.; Boschman, L.; Hoekstra, S.

    2015-01-14

    We have investigated the photoionization and photodissociation of free coronene cations C{sub 24}H{sub 12}{sup +} upon soft X-ray photoabsorption in the carbon K-edge region by means of a time-of-flight mass spectrometry approach. Core excitation into an unoccupied molecular orbital (below threshold) and core ionization into the continuum both leave a C 1s vacancy, that is subsequently filled in an Auger-type process. The resulting coronene dications and trications are internally excited and cool down predominantly by means of hydrogen emission. Density functional theory was employed to determine the dissociation energies for subsequent neutral hydrogen loss. A statistical cascade model incorporating these dissociation energies agrees well with the experimentally observed dehydrogenation. For double ionization, i.e., formation of intermediate C{sub 24}H{sub 12}{sup 3+⋆}trications, the experimental data hint at loss of H{sup +} ions. This asymmetric fission channel is associated with hot intermediates, whereas colder intermediates predominantly decay via neutral H loss.

  5. Microwave absorption measurements of melting spherical and nonspherical hydrometeors

    NASA Technical Reports Server (NTRS)

    Hansman, R. J., Jr.

    1986-01-01

    Measurements were made of the absorption behavior of melting and freezing hydrometeors using resonant cavity perturbation techniques at a wavelength of 2.82 cm. Melting ice spheres with equivalent melted diameters between 1.15 and 2.00 mm exhibit a period of strong absorption during melting as predicted by prior theoretical calculations. However, the measured magnitude of the absorption peak exceeds the predicted value. Absorption measuremets of melting oblate and prolate ice ellipsoids also exhibit enhanced absorption during melting.

  6. In vivo absorption spectroscopy for absolute measurement.

    PubMed

    Furukawa, Hiromitsu; Fukuda, Takashi

    2012-10-01

    In in vivo spectroscopy, there are differences between individual subjects in parameters such as tissue scattering and sample concentration. We propose a method that can provide the absolute value of a particular substance concentration, independent of these individual differences. Thus, it is not necessary to use the typical statistical calibration curve, which assumes an average level of scattering and an averaged concentration over individual subjects. This method is expected to greatly reduce the difficulties encountered during in vivo measurements. As an example, for in vivo absorption spectroscopy, the method was applied to the reflectance measurement in retinal vessels to monitor their oxygen saturation levels. This method was then validated by applying it to the tissue phantom under a variety of absorbance values and scattering efficiencies.

  7. Low-resolution continuum source simultaneous multi-element electrothermal atomic absorption spectrometry: steps into practice

    NASA Astrophysics Data System (ADS)

    Katskov, Dmitri

    2015-03-01

    The theory and practical problems of continuum source simultaneous multi-element electrothermal atomic absorption spectrometry (SMET AAS) are discussed by the example of direct analysis of underground water. The experimental methodology is based on pulse vaporization of the sample in a fast heated graphite tube and measurement of transient absorption of continuum spectrum radiation from D2 and Xe lamps within 200-400 nm wavelengths range with a low resolution spectral instrument and linear charge-coupled device. The setup permits the acquisition of 200 spectra during 1 s atomization pulse. Respective data matrix absorbance vs wavelength/time is employed for the quantification of elements in the sample. The calculation algorithm developed includes broad band and continuum background correction, linearization of function absorbance vs. concentration of atomic vapor and integration of thus modified absorbance at the resonance lines of the elements to be determined. Practical application shows that the method can be employed for the direct simultaneous determination of about 20 elements above microgram per liter level within 3-5 orders of the magnitude concentration range. The investigated sources of measurement errors are mainly associated with the atomization and vapor transportation problems, which are aggravated for the simultaneous release of major and minor sample constituents. Respective corrections concerning the selection of analytical lines, optimal sampling volume, matrix modification and cleaning of the atomizer have been introduced in the SMET AAS analytical technology. Under the optimized experimental conditions the calibration curves in Log-Log coordinates for all the investigated analytes in the single or multi-element reference solutions are approximated by the first order equations. The use of these equations as permanent characteristics of the setup enables instant quantification of Al, Ca, Co, Cr, Cu, Fe, Mg, Mn and Ni in the underground water

  8. Optimization of electrothermal atomization parameters for simultaneous multielement atomic absorption spectrometry

    USGS Publications Warehouse

    Harnly, J.M.; Kane, J.S.

    1984-01-01

    The effect of the acid matrix, the measurement mode (height or area), the atomizer surface (unpyrolyzed and pyrolyzed graphite), the atomization mode (from the wall or from a platform), and the atomization temperature on the simultaneous electrothermal atomization of Co, Cr, Cu, Fe, Mn, Mo, Ni, V, and Zn was examined. The 5% HNO3 matrix gave rise to severe irreproducibility using a pyrolyzed tube unless the tube was properly "prepared". The 5% HCl matrix did not exhibit this problem, and no problems were observed with either matrix using an unpyrolized tube or a pyrolyzed platform. The 5% HCl matrix gave better sensitivities with a pyrolyzed tube but the two matrices were comparable for atomization from a platform. If Mo and V are to be analyzed with the other seven elements, a high atomization temperature (2700??C or greater) is necessary regardless of the matrix, the measurement mode, the atomization mode, or the atomizer surface. Simultaneous detection limits (peak height with pyrolyzed tube atomization) were comparable to those of conventional atomic absorption spectrometry using electrothermal atomization above 280 nm. Accuracies and precisions of ??10-15% were found in the 10 to 120 ng mL-1 range for the analysis of NBS acidified water standards.

  9. Determination of nickel, chromium and cobalt in wheat flour using slurry sampling electrothermal atomic absorption spectrometry.

    PubMed

    González, M; Gallego, M; Valcárcel, M

    1999-05-01

    The slurry technique was applied to the determination of Ni, Cr and Co in wheat flour by electrothermal atomic absorption spectrometry (ETAAS). The influence of the graphite furnace temperature programme was optimized. Optimum sensitivity was obtained by using a mixture of 15% HNO(3)-10% H(2)O(2) as suspended medium for a 3% w/v slurry in the determination of Ni; lower concentrations of HNO(3) were necessary for the determination of Co and Cr (viz. 5 and 10%). The precision of direct analyses of the slurries was improved by using mechanical agitation between measurements; thus, the RSD of the measurements was ca. 5% for repeatability. The direct slurry sampling (SS) technique is suitable for the determination of Ni and Cr in wheat flour samples at levels of 150-450 and 30-72 ng g(-1), respectively, as it provides results similar to those obtained by ashing the sample. However, the typically low level of Co in these samples precluded its determination by the proposed method (the study was made in an SRM spiked wholemeal flour), at least in those samples that were contaminated with elevated concentrations of the metal (viz. more than 90 ng of Co per g of flour). The method provides a relative standard deviation of 6, 8, and 4% for Ni, Cr, and Co, respectively.

  10. ABSORPTION MEASURE DISTRIBUTION IN Mrk 509

    SciTech Connect

    Adhikari, T. P.; Różańska, A.; Sobolewska, M.; Czerny, B.

    2015-12-20

    In this paper we model the observed absorption measure distribution (AMD) in Mrk 509, which spans three orders of magnitude in ionization level with a single-zone absorber in pressure equilibrium. AMD is usually constructed from observations of narrow absorption lines in radio-quiet active galaxies with warm absorbers. We study the properties of the warm absorber in Mrk 509 using recently published broadband spectral energy distribution observed with different instruments. This spectrum is an input in radiative transfer computations with full photoionization treatment using the titan code. We show that the simplest way to fully reproduce the shape of AMD is to assume that the warm absorber is a single zone under constant total pressure. With this assumption, we found theoretical AMD that matches the observed AMD determined on the basis of the 600 ks reflection grating spectrometer XMM-Newton spectrum of Mrk 509. The softness of the source spectrum and the important role of the free–free emission breaks the usual degeneracy in the ionization state calculations, and the explicit dependence of the depths of AMD dips on density open a new path to the density diagnostic for the warm absorber. In Mrk 509, the implied density is of the order of 10{sup 8} cm{sup −3}.

  11. Atmospheric Measurements by Cavity Enhanced Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Yi, Hongming; Wu, Tao; Coeur-Tourneur, Cécile; Fertein, Eric; Gao, Xiaoming; Zhao, Weixiong; Zhang, Weijun; Chen, Weidong

    2015-04-01

    Since the last decade, atmospheric environmental monitoring has benefited from the development of novel spectroscopic measurement techniques owing to the significant breakthroughs in photonic technology from the UV to the infrared spectral domain [1]. In this presentation, we will overview our recent development and applications of cavity enhanced absorption spectroscopy techniques for in situ optical monitoring of chemically reactive atmospheric species (such as HONO, NO3, NO2, N2O5) in intensive campaigns [2] and/or in smog chamber studies [3]. These field deployments demonstrated that modern photonic technologies (newly emergent light sources combined with high sensitivity spectroscopic techniques) can provide a useful tool to improve our understanding of tropospheric chemical processes which affect climate, air quality, and the spread of pollution. Experimental detail and preliminary results will be presented. Acknowledgements. The financial support from the French Agence Nationale de la Recherche (ANR) under the NexCILAS (ANR-11-NS09-0002) and the CaPPA (ANR-10-LABX-005) contracts is acknowledged. References [1] X. Cui, C. Lengignon, T. Wu, W. Zhao, G. Wysocki, E. Fertein, C. Coeur, A. Cassez,L. Croisé, W. Chen, et al., "Photonic Sensing of the Atmosphere by absorption spectroscopy", J. Quant. Spectrosc. Rad. Transfer 113 (2012) 1300-1316 [2] T. Wu, Q. Zha, W. Chen, Z. XU, T. Wang, X. He, "Development and deployment of a cavity enhanced UV-LED spectrometer for measurements of atmospheric HONO and NO2 in Hong Kong", Atmos. Environ. 95 (2014) 544-551 [3] T. Wu, C. Coeur-Tourneur, G. Dhont,A. Cassez, E. Fertein, X. He, W. Chen,"Application of IBBCEAS to kinetic study of NO3 radical formation from O3 + NO2 reaction in an atmospheric simulation chamber", J. Quant. Spectrosc. Rad. Transfer 133 (2014)199-205

  12. Literature study of microwave-assisted digestion using electrothermal atomic absorption spectrometry.

    PubMed

    Chakraborty, R; Das, A K; Cervera, M L; De La Guardia, M

    1996-05-01

    The literature on the use of microwave-assisted digestion procedures for subsequent sample analysis by means of electrothermal atomic absorption spectrometry (ETAAS) is reviewed. The literature survey reveals that this digestion technique has been applied mainly for biological materials. The elements most extensively determined by this method are cadmium and lead followed by copper, chromium, nickel and iron. The microwave digestion conditions, ETAAS furnace programmes and analytical details of the developed methodologies have been carefully revised.

  13. Recent developments in atomizers for electrothermal atomic absorption spectrometry.

    PubMed

    Frech, W

    1996-06-01

    This review first describes general requirements to be met for suitable base materials used to produce electrothermal atomizers (ETAs). In this connection the physical and chemical properties of adequate types of graphite and metals are discussed. Further, various atomizer designs, their temperature dynamics during atomization and general performance characteristics are critically reviewed. For end-heated Massmann-type atomizers, discussions are focused on recent developments of, e.g., contoured tubes to achieve improved temperature homogeneity over the tube length, second surface atomizers to realize temporally isothermal atomization and tubes with graphite filters to reduce interference effects. The state-of-the-art of platform equipped, side-heated atomizers with integrated contacting bridges are characterized mainly with respect to heating dynamics, as well as susceptibility to interference- and memory effects. In contrast to end-heated ETAs, the tube ends of side-heated ETAs are freely located in the furnace compartment and, as a consequence of this configuration, convective gas flows can easily appear. The magnitude and effect of these flows on analytical performance are discussed and measures are suggested, permitting operation under diffusion controlled conditions. A critical comparison of classical constant temperature atomizers with state-of-the-art platform equipped ETAs is made and from this it is concluded that future ETA developments are likely to involve only minor modifications aiming at, e.g., the reduction of cycling times or the improvement of tube surface properties.

  14. Liquid phase microextraction and ultratrace determination of cadmium by modified graphite furnace atomic absorption spectrometry.

    PubMed

    Nazari, Saeid

    2009-06-15

    A powerful microextraction technique was used for determination of cadmium in water samples using liquid phase microextraction (LPME) followed by graphite furnace atomic absorption spectrometry (GF-AAS). In a preconcentration step, cadmium was extracted from a 2 ml of its aqueous sample in the pH 7 as 5,7-dibromoquinoline-8-ol (DBQ) complex into a 4 microl drop of benzyl alcohol. After extraction, the micro drop was retracted and directly transferred into a graphite tube modified by [W.Rh.Pd](c). Some effective parameters on extraction and complex formation, such as type and volume of organic solvent, pH, concentration of chelating agent, extraction time and stirring rate were optimized. Under the optimum conditions, the enrichment factor and recovery were 450% and 90%, respectively. The calibration graph was linear in the range of 0.008-1 microg L(-1) with correlation coefficient of 0.9961 under the optimum conditions of the recommended procedure. The detection limit based on the 3Sb criterion was 0.0035 microg L(-1) and relative standard deviation (RSD) for eight replicate measurement of 0.1 microg L(-1) and 0.4 microg L(-1) cadmium was 5.2% and 4.5%, respectively. The characteristic concentration was 0.0032 microg L(-1) equivalent to a characteristic mass of 12.8 fg. In order to evaluate the accuracy and recovery of the presented method the procedure was applied to the analysis of reference materials and seawater.

  15. Determination of silicon in serum and urine by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Huang, Zhuo-er

    1995-09-01

    A sensitive, simple and accurate method for the routine determination of trace silicon in serum and urine by Zeeman electrothermal atomic absorption spectrometry is described. The samples are directly determined after 20-fold dilution of serum and 100-fold dilution of urine. No L'vov platform is used. The signal enhancement of silicon atomization in pyrolytic graphite coated graphite tubes is achieved by using a mixture of calcium chloride and lanthanum nitrate as chemical modifier. The interferences arising from the biological matrices have been eliminated by the addition of ammonium dihydrogenphosphate in the sample solutions. The aqueous calibration curve is linear to at least 300 μg l -1, the characteristic mass is 37 pg (integrated absorbance signal), whereas the detection limit (3SD) is 1.5 μg l -1 for silicon in both diluted serum and urine samples. The recoveries of silicon added to the diluted samples are 101 ± 1.8% for sera and 98.2 ± 3.5% for the urine specimens, independent of the dilution ratio. The silicon measurement results for the serum and urine from healthy adults and for the serum from the patients with chronic renal failure on hemodialysis are presented.

  16. Determination of total gaseous lead in the atmosphere by honeycomb denuder/electrothermal atomic absorption spectrometry.

    PubMed

    Zhang, Bicheng; Wu, Tao; Yu, Jimmy C

    2005-09-01

    A technique is described for the determination of total gaseous lead in the atmosphere by honeycomb denuder collection, followed by an electrothermal atomic absorption spectrometry (ETAAS) measurement. The collection efficiency of the honeycomb denuder in which a solution containing 2% HNO3/2% glycerine/1% ammonium dihydrogenphosphate was coated for trapping the gaseous lead in the atmosphere was 98.8%. The linear absorbance response was obtained for a concentration range of 0-1.39 microg m(-3) of lead in the atmosphere. A precision of 4.8% RSD (peak-height absorbance, n = 11) for an aqueous solution of 1 ng of lead standard, characteristic masses (CM) of 23 pg and detection limit (3sigma) of 54 pg for an aqueous solution of 0.01 ng lead standard was achieved with 100 microg ammonium dihydrogenphosphate as a chemical modifier. The average recovery of lead in three standard samples prepared by the independent digestion of NIST SRM 1648 (Urban Particulate Matter) using our analytical system was 97.8%. The total content of the gaseous lead in the atmosphere of our laboratories was 0.35-0.38 microg m(-3).

  17. Determination of some antihistaminic drugs by atomic absorption spectrometry and colorimetric methods.

    PubMed

    El-Kousy, N; Bebawy, L I

    1999-08-01

    Atomic absorption spectrometry (AAS) and colourimetric methods have been developed for the determination of pizotifen (I), ketotifen (II) and loratadine (III). The first method depends on the reaction of the three drugs (I); (II) and (III) with cobalt thiocyanate reagent at pH 2 to give ternary complexes. These complexes are readily extracted with organic solvent and estimated by indirect atomic absorption method via the determination of the cobalt content in the formed complex after extraction in 0.1 M hydrochloric acid. It was found that the three drugs can be determined in the concentration ranges from 10 to 74, 12 to 95 and 10 to 93 microg ml(-1) with mean percentage recovery of 99.71+/-0.87, 99.70+/-0.79 and 99.62+/-0.75%, respectively. The second method is based on the formation of orange red ion pairs as a result of the reaction between (I); (II) and (III) and molybdenum thiocyanate with maximum absorption at 469.5 nm in dichloromethane. Appropriate conditions were established for the colour reaction. Under the proposed conditions linearity was obeyed in the concentration ranges 3.5-25, 5-37.5 and 2.5-22.5 microg ml(-1) with mean percentage recovery of 99.60+/-0.41, 100.11+/-0.43 and 99.31+/-0.47% for (I): (II) and (III), respectively. The third method depends on the formation of radical ion using 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ). The colour formed was measured at 588 nm for the three drugs (I); (II) and (III), respectively. The method is valid in concentration range 10-80 microg ml(-1) with mean percentage recovery 99.75+/-0.44, 99.94+/-0.72 and 99.17+/-0.36% for (I); (II) and (III), respectively. The proposed methods were applied to the analysis of pharmaceutical preparations. The results obtained were statistically analysed and compared with those obtained by applying the official and reference methods.

  18. Molar Absorptivity Measurements in Absorbing Solvents: Impact on Solvent Absorptivity Values.

    PubMed

    Bohman, Ariel; Arnold, Mark A

    2016-10-18

    Molar absorptivity is a fundamental molecular property that quantifies absorption strength as a function of wavelength. Absolute measurements of molar absorptivity demand accounting for all mechanisms of light attenuation, including reflective losses at interfaces associated with the sample. Ideally, such measurements are performed in nonabsorbing solvents and reflective losses can be determined in a straightforward manner from Fresnel equations or effectively accounted for by path length difference methods. At near-infrared wavelengths, however, many solvents, including water, are absorbing which complicates the quantification of reflective losses. Here, generalized equations are developed for calculating absolute molar absorptivities of neat liquids wherein the dependency of reflective loss on absorption properties of the liquid are considered explicitly. The resulting equations are used to characterize sensitivity of absolute molar absorptivity measurements for solvents to the absorption strength of the solvent as well as the path length of the measurement. Methods are derived from these equations to properly account for reflective losses in general and the effectiveness of these methods is demonstrated for absolute molar absorptivity measurements for water over the combination region (5000-4000 cm(-1)) of the near-infrared spectrum. Results indicate that ignoring solvent absorption effects can incorporate wide ranging systematic errors depending upon experimental conditions. As an example, systematic errors range from 0 to 10% for common conditions used in the measurement of absolute molar absorptivity of water over the combination region of the near-infrared spectrum.

  19. Atmospheric particulate absorption and black carbon measurement.

    PubMed

    Lindberg, J D; Douglass, R E; Garvey, D M

    1999-04-20

    It is convenient to measure the optical attenuation A of the combination of a layer of atmospheric particulate matter and the quartz fiber filter on which it has been collected. The problem of relating A to the absorption and scattering coefficients k and s of the particulate matter itself is treated as a problem in diffuse reflectance spectroscopy using the KubelkaMunk theory. The results show that although, in general, A is a nonlinear function strongly dependent on both s and k, for a limited range of s and sample thickness d, A can be a practically linear function of k. Fortunately, this range includes that common to atmospheric particulate samples. Furthermore, it is shown that if the filter's reflectance is sufficiently high, A can be nearly independent of s. This is in agreement with experimental and, for the limiting case when the substrate filter reflectance is unity, theoretical results obtained by other researchers. Use of such measurements of A as a means of determining the black carbon mass loading C on a filter is also investigated. It is shown that when the black carbon mass fraction f(c) is high, as it is for samples collected in large urban areas, A is a predictable and practically linear function of C. However, when f(c) is low, as it is for many rural locations, then the slope of the function A(C) is strongly dependent on f(c), leading to possible overestimates of C. This problem can be alleviated by making the measurement of A at near-infrared wavelengths rather than in the visible spectrum.

  20. Flame and graphite furnace atomic absorption spectrometry for trace element determination in vegetable oils, margarine and butter after sample emulsification.

    PubMed

    Ieggli, C V S; Bohrer, D; Do Nascimento, P C; De Carvalho, L M

    2011-05-01

    Trace element analysis plays an important role in oil characterisation and in the detection of oil adulteration because the quality of edible oils and fats is affected by their trace metal content. In this study, the quantification of selected metals in various oils and fats (rice oil, canola oil, sunflower oil, corn oil, soy oil, olive oil, light margarine, regular margarine and butter) was carried out using flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after sample emulsification. FAAS was used to determine the Na, K, Ca, Mg, Zn and Fe levels in the samples, while GFAAS was used for quantifying Cr, Ni, As, Pb, Cd, Cu and Mn, as these elements appeared in the samples at much lower concentrations. Tween-80 and Triton X-100 were employed as surfactants, and emulsions were prepared by a conventional method that involved heating and mixing of the constituents. Complete stabilisation was achieved through magnetic stirring for 15 min at room temperature. The evaluated figures of merit were linearity, accuracy and sensitivity, which were determined by the characteristic concentration and mass. Analysis of spiked samples demonstrated accuracy, which ranged from 90% (Na) to 112% (Fe) for FAAS and from 83% (Cd) to 121% (Pb) for GFAAS measurements. Atomic absorption spectrometry proved to be a promising approach for the analysis of metals in emulsified edible oils and fats. Additionally, under appropriate emulsification conditions (formulation, stirring time and temperature), the emulsions were homogeneous, had excellent stability, and had appropriate viscosity. The proposed method has proved to be simple, sensitive, reproducible, and economical.

  1. Quantification of the fluorine containing drug 5-fluorouracil in cancer cells by GaF molecular absorption via high-resolution continuum source molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Krüger, Magnus; Huang, Mao-Dong; Becker-Roß, Helmut; Florek, Stefan; Ott, Ingo; Gust, Ronald

    The development of high-resolution continuum source molecular absorption spectrometry made the quantification of fluorine feasible by measuring the molecular absorption as gallium monofluoride (GaF). Using this new technique, we developed on the example of 5-fluorouracil (5-FU) a graphite furnace method to quantify fluorine in organic molecules. The effect of 5-FU on the generation of the diatomic GaF molecule was investigated. The experimental conditions such as gallium nitrate amount, temperature program, interfering anions (represented as corresponding acids) and calibration for the determination of 5-FU in standard solution and in cellular matrix samples were investigated and optimized. The sample matrix showed no effect on the sensitivity of GaF molecular absorption. A simple calibration curve using an inorganic sodium fluoride solution can conveniently be used for the calibration. The described method is sensitive and the achievable limit of detection is 0.23 ng of 5-FU. In order to establish the concept of "fluorine as a probe in medicinal chemistry" an exemplary application was selected, in which the developed method was successfully demonstrated by performing cellular uptake studies of the 5-FU in human colon carcinoma cells.

  2. Calculating Measurement Uncertainties for Mass Spectrometry Data

    NASA Astrophysics Data System (ADS)

    Essex, R. M.; Goldberg, S. A.

    2006-12-01

    A complete and transparent characterization of measurement uncertainty is fundamentally important to the interpretation of analytical results. We have observed that the calculation and reporting of uncertainty estimates for isotopic measurement from a variety of analytical facilities are inconsistent, making it difficult to compare and evaluate data. Therefore, we recommend an approach to uncertainty estimation that has been adopted by both US national metrology facilities and is becoming widely accepted within the analytical community. This approach is outlined in the ISO "Guide to the Expression of Uncertainty in Measurement" (GUM). The GUM approach to uncertainty estimation includes four major steps: 1) Specify the measurand; 2) Identify uncertainty sources; 3) Quantify components by determining the standard uncertainty (u) for each component; and 4) Calculate combined standard uncertainty (u_c) by using established propagation laws to combine the various components. To obtain a desired confidence level, the combined standard uncertainty is multiplied by a coverage factor (k) to yield an expanded uncertainty (U). To be consistent with the GUM principles, it is also necessary create an uncertainty budget, which is a listing of all the components comprising the uncertainty and their relative contribution to the combined standard uncertainty. In mass spectrometry, Step 1 is normally the determination of an isotopic ratio for a particular element. Step 2 requires the identification of the many potential sources of measurement variability and bias including: gain, baseline, cup efficiency, Schottky noise, counting statistics, CRM uncertainties, yield calibrations, linearity calibrations, run conditions, and filament geometry. Then an equation expressing the relationship of all of the components to the measurement value must be written. To complete Step 3, these potential sources of uncertainty must be characterized (Type A or Type B) and quantified. This information

  3. Total Absorption Gamma-ray Spectrometer (TAGS) Intensity Distributions from INL's Gamma-Ray Spectrometry Center

    DOE Data Explorer

    Greenwood, R. E.

    A 252Cf fission-product source and the INL on-line isotope separator were used to supply isotope-separated fission-product nuclides to a total absorption -ray spectrometer. This spectrometer consisted of a large (25.4-cm diameter x 30.5-cm long) NaI(Tl) detector with a 20.3-cm deep axial well in which is placed a 300-mm2 x 1.0-mm Si detector. The spectra from the NaI(Tl) detector are collected both in the singles mode and in coincidence with the B-events detected in the Si detector. Ideally, this detector would sum all the energy of the B- rays in each cascade following the population of daughter level by B- decay, so that the event could be directly associated with a particular daughter level. However, there are losses of energy from attenuation of the rays before they reach the detector, transmission of rays through the detector, escape of secondary photons from Compton scattering, escape of rays through the detector well, internal conversion, etc., and the measured spectra are thus more complicated than the ideal case and the analysis is more complex. Analysis methods have been developed to simulate all of these processes and thus provide a direct measure of the B- intensity distribution as a function of the excitation energy in the daughter nucleus. These data yield more accurate information on the B- distribution than conventional decay-scheme studies for complex decay schemes with large decay energies, because in the latter there are generally many unobserved and observed but unplaced rays. The TAGS data have been analyzed and published [R. E. Greenwood et al., Nucl Instr. and metho. A390(1997)] for 40 fission product-nuclides to determine the B- intensity distributions. [Copied from the TAGS page at http://www.inl.gov/gammaray/spectrometry/tags.shtml]. Those values are listed on this page for quick reference.

  4. Feasibility of filter atomization in high-resolution continuum source atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Heitmann, Uwe; Becker-Ross, Helmut; Katskov, Dmitri

    2006-03-01

    A prototype spectrometer for high-resolution continuum source atomic absorption spectrometry (HR-CS AAS), built at ISAS Berlin, Germany, was combined with a graphite filter atomizer (GFA), earlier developed at TUT, Pretoria, South Africa. The furnace and auto-sampler units from a commercial AA spectrometer, model AAS vario 6 (Analytik Jena AG, Jena, Germany), were employed in the instrument. Instead of conventional platform tube, the GFA was used to provide low measurement susceptibility to interferences and short determination cycle. The GFA was modified according to the design of the furnace unit and optimal physical parameters of its components (filter and collector) found. Afterwards, optimal GFA was replicated and tested to outline analytical performances of the HR-CS GFA AA spectrometer in view of prospects of multi-element analysis. In particular, reproducibility of performances, repeatability of analytical signals, lifetime, temperature limit and duration of the measurement cycle were examined, and elements available for determination justified. The results show that the peak area of the atomic absorption signal is reproduced in various GFA copies within ± 4% deviation range. The GFA can stand temperatures of 2800 °C with 6 s hold time for 55 temperature cycles, and 2700 °C (8 s) for about 200 cycles. Only the external tube is prone to destruction while the filter and collector do not show any sign of erosion caused by temperature or aggressive matrix. Analytical signals are affected insignificantly by tube aging. Repeatability of the peak area remains within 1.1-1.7% RSD over more than hundred determination cycles. Peak areas are proportional to the sample volume of injected organic and inorganic liquids up to at least 50 μL. The drying stage is combined with hot sampling and cut down to 15-20 s. The list of metals available for determination with full vapor release includes Al, Co, Cr, Ni, Pt as well as more volatile metals. Characteristic masses at

  5. Automation of preparation of nonmetallic samples for analysis by atomic absorption and inductively coupled plasma spectrometry

    NASA Technical Reports Server (NTRS)

    Wittmann, A.; Willay, G.

    1986-01-01

    For a rapid preparation of solutions intended for analysis by inductively coupled plasma emission spectrometry or atomic absorption spectrometry, an automatic device called Plasmasol was developed. This apparatus used the property of nonwettability of glassy C to fuse the sample in an appropriate flux. The sample-flux mixture is placed in a composite crucible, then heated at high temperature, swirled until full dissolution is achieved, and then poured into a water-filled beaker. After acid addition, dissolution of the melt, and filling to the mark, the solution is ready for analysis. The analytical results obtained, either for oxide samples or for prereduced iron ores show that the solutions prepared with this device are undistinguished from those obtained by manual dissolutions done by acid digestion or by high temperature fusion. Preparation reproducibility and analytical tests illustrate the performance of Plasmasol.

  6. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Krawczyk, Magdalena

    2007-03-01

    The analytical performance of coupled hydride generation — integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H 2Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements (a water-cooled single silica tube, double-slotted quartz tube or an "integrated trap") was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3 σ), was 0.9 ng mL - 1 for Te. For a 2 min in situ pre-concentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation — atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% ( n = 6) for Te. The designs studied include slotted tube, single silica tube and integrated atom trap-cooled atom traps. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  7. Determination of mercury distribution inside spent compact fluorescent lamps by atomic absorption spectrometry

    SciTech Connect

    Rey-Raap, Natalia

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer New treatments for CFL are required considering the aim of Directive 202/96/CE. Black-Right-Pointing-Pointer It is shown that most of the mercury introduced into a CFL is in the phosphor powder. Black-Right-Pointing-Pointer Experimental conditions for microwave-assisted sample digestion followed by AAS measurements are described. Black-Right-Pointing-Pointer By washing the glass it is possible to reduce the concentration below legal limits. - Abstract: In this study, spent compact fluorescent lamps were characterized to determine the distribution of mercury. The procedure used in this research allowed mercury to be extracted in the vapor phase, from the phosphor powder, and the glass matrix. Mercury concentration in the three phases was determined by the method known as cold vapor atomic absorption spectrometry. Median values obtained in the study showed that a compact fluorescent lamp contained 24.52 {+-} 0.4 ppb of mercury in the vapor phase, 204.16 {+-} 8.9 ppb of mercury in the phosphor powder, and 18.74 {+-} 0.5 ppb of mercury in the glass matrix. There are differences in mercury concentration between the lamps since the year of manufacture or the hours of operation affect both mercury content and its distribution. The 85.76% of the mercury introduced into a compact fluorescent lamp becomes a component of the phosphor powder, while more than 13.66% is diffused through the glass matrix. By washing and eliminating all phosphor powder attached to the glass surface it is possible to classified the glass as a non-hazardous waste.

  8. Evaluation of propolis polyphenols absorption in humans by liquid chromatography/tandem mass spectrometry.

    PubMed

    Gardana, Claudio; Simonetti, Paolo; Berti, Cristiana; Pietta, Piergiorgio

    2007-01-01

    Propolis has various biological activities such as antibacterial, antiviral, antioxidant, immunostimulating and antiinflammatory, which are generally ascribed to the polyphenolic fraction. The aim of this study was to evaluate the absorption of the main polyphenols [caffeic acid (CA), pinobanksin-5methyl ether (P-5ME), pinobanksin (Pb), chrysin (C), pinocembrin (P), galangin (G), pinobanksin-3-acetate, pinobanksin esters and caffeic acid phenylethyl ester (CAPE)] from a dewaxed and standardized extract of propolis (EPID). Fifteen healthy volunteers consumed 5 mL EPID in water, corresponding to 125 mg of flavonoids. Blood samples were collected before, each hour for 8 h and 24 h after EPID intake. After deconjugation by beta-glucuronidase/sulfatase the plasma samples were analyzed by a selective liquid chromatography/tandem mass spectrometry (LC/MS/MS) method using morin as internal standard (I.S.). A kinetic profile characterized by two t(max), respectively at 1 h and about 5 h post-ingestion, was observed in all the subjects. The two peaks may be due to enterohepatic cycling. Among the various polyphenols ingested, only P-5ME, Pb, C, P and G were detected in plasma and C(max)t(1h) were 65.7 +/- 13.3, 46.5 +/- 12.7, 79.5 +/- 18.6, 168.1 +/- 16.3 and 113.7 +/- 16.8 ng/mL, respectively. These levels decreased significantly after 8 h and were no longer detectable 24 h after EPID intake. The recovery of the extraction for CA, Pb, C, P, G and I.S. from spiked plasma was 95.2 +/- 3.1, 93.1 +/- 3.6, 91 +/- 2.5, 96.4 +/- 4.2, 93.4 +/- 2.4 and 85.5 +/- 2.4%, respectively. The results of this study evidence that flavonoids from EPID are absorbed, metabolized and Pb-5ME and G seem to have apparent absorption, measured as (AUC/dose), higher than C, P and Pb.

  9. [Determination of calcium and magnesium in wheat flour by suspension sampling-flame atomic absorption spectrometry].

    PubMed

    Liu, L; Zhang, Q; Hu, Y

    1999-06-01

    Suspension sampling technique was applied to flame atomic absorption spectrometry and was successfully used to determine calcium and magnesium in wheat flour. The wheat flour was suspended in agar sol containing dibutyl phthalate and made into suspension. Choice of suspension agent and elimination of chemical interference were studied. The test solution was injected into air-acetylene flame to determine calcium and magnesium by standard addition method. Determination results were consistent with those obtained by ashing method. The t-test showed that no difference was found between the two methods. Displacement of ashing method by suspension sampling method for the sample pretreatment is possible. This method is convenient, rapid and accurate.

  10. Determination of mercury in sewage sludge by direct slurry sampling graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Baralkiewicz, Danuta; Gramowska, Hanka; Kózka, Małgorzata; Kanecka, Anetta

    2005-03-01

    Ultrasonic slurry sampling electrothermal atomic absorption spectrometry (ETAAS) method was elaborated to the determination of Hg in sewage sludge samples with the use of KMnO 4+Pd modifier. The minimum sample amount required for slurry preparation with respect to sample homogeneity was evaluated by weighting masses between 3 and 30 mg directly into the autosampler cups. Validation of the proposed method was performed with the use of Certified Reference Materials of sewage sludge, CRM 007-040 and CRM 144R. Two sewage sludge samples from Poznañ (Poland) city were analysed using the present direct method and a method with sample digestion, resulting in no difference within statistical error.

  11. Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

    2016-12-01

    The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

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

    PubMed

    Chen, Li-dan; Chen, Kai-kao

    2012-01-01

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

  13. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    NASA Astrophysics Data System (ADS)

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R.; Welz, Bernhard; Carasek, Eduardo; de Andrade, Jailson B.

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%).

  14. Isotope ratio measurements by secondary ion mass spectrometry (SIMS) and glow discharge mass spectrometry (GDMS)

    NASA Astrophysics Data System (ADS)

    Betti, Maria

    2005-04-01

    The basic principles of secondary ion mass spectrometry and glow discharge mass spectrometry have been shortly revisited. The applications of both techniques as exploited for the isotope ratio measurements in several matrices have been reviewed. Emphasis has been given to research fields in expansions such as solar system studies, medicine, biology, environment and nuclear forensic. The characteristics of the two techniques are discussed in terms of sensitivity and methodology of quantification. Considerations on the different detection possibilities in SIMS are also presented.

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

    NASA Astrophysics Data System (ADS)

    Berndt, R.; Mortreau, P.

    2011-07-01

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

  16. Examination of the Measurement of Absorption Using the Reverberant Room Method for Highly Absorptive Acoustic Foam

    NASA Technical Reports Server (NTRS)

    Hughes, William O.; McNelis, Anne M.; Chris Nottoli; Eric Wolfram

    2015-01-01

    The absorption coefficient for material specimens are needed to quantify the expected acoustic performance of that material in its actual usage and environment. The ASTM C423-09a standard, "Standard Test Method for Sound Absorption and Sound Absorption Coefficients by the Reverberant Room Method" is often used to measure the absorption coefficient of material test specimens. This method has its basics in the Sabine formula. Although widely used, the interpretation of these measurements are a topic of interest. For example, in certain cases the measured Sabine absorption coefficients are greater than 1.0 for highly absorptive materials. This is often attributed to the diffraction edge effect phenomenon. An investigative test program to measure the absorption properties of highly absorbent melamine foam has been performed at the Riverbank Acoustical Laboratories. This paper will present and discuss the test results relating to the effect of the test materials' surface area, thickness and edge sealing conditions. A follow-on paper is envisioned that will present and discuss the results relating to the spacing between multiple piece specimens, and the mounting condition of the test specimen.

  17. Temporal and spatial temperature distributions in transversely heated graphite tube atomizers and their analytical characteristics for atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Sperling, Michael; Welz, Bernard; Hertzberg, Joachim; Rieck, Christof; Marowsky, Gerd

    1996-07-01

    The important role which temperature plays in atomic absorption spectrometry (AAS) for the formation and detection of atoms in the absorption volume is discussed and the literature is reviewed. Non-homogeneous temperature distribution in the absorption volume is in contradiction to one of the prerequisites for the application of Beer's law used in AAS to convert absorbance into analyte concentration or mass, and is particularly troublesome for an "absolute analysis" envisaged for electrothermal atomic absorption spectrometry (ETAAS). Coherent anti-Stokes Raman scattering (CARS) is used to study the gas-phase temperature distribution in a state-of-the-art transversely heated graphite tube atomizer (THGA). The effect of the internal gas flow on the size of the heated atmosphere is studied by steady-state temperature measurements. Temporally and spatially resolved measurements make it possible to study the temperature field within the atomizer volume in all three dimensions during the rapid heating of the furnace to final temperatures in the range 2173-2673 K. The role of the integrated platform of the THGA on the temperature field is investigated by temperature measurements of the gas phase in the presence and absence of the platform. The platform is identified as the major source of temperature gradients inside the tube volume, which may be as high as 1000 K in the radial direction during rapid heating. These gradients are most pronounced for heating cycles starting at room temperature and gradually decrease with increasing starting temperature. Shortly after the tube wall reaches its final temperature, the gas-phase temperature equilibrates and approaches the wall temperature. Because of the unavoidable contact with the cold environment at the open ends of the tube, minor temperature gradients are observed in the gas phase also in longitudinal direction, which can be further reduced by restricting the openings with end caps. The results obtained for the THGA are

  18. Determination of occupational exposure to organotin compounds after multivariate optimization of a liquid chromatography flame atomic absorption spectrometry system

    NASA Astrophysics Data System (ADS)

    Nygren, Olle

    1993-07-01

    The detection limit, obtained with a previously developed liquid chromatography flame atomic absorption spectrometry system, was not low enough for the determination of occupational exposure to organotin compounds. Optimization of the system was thus necessary. Many experimental factors may influence the response of the system, and interaction effects between these parameters may also be expected. With optimization by multivariate methods, the response of the system was improved and a 2.5-times better detection limit for organotin compounds was obtained, which was adequate for determination of occupational exposure. The system was employed for determination of occupational exposure to organotin-based wood preservatives at an impregnation plant. No exposure to butyltin compounds above 1/10 of the threshold limit value could be measured at any sampling place. It was also found that up to 30% of the tributyltin in impregnation solutions in use was dealkylated to less fungitoxic dibutyltin compounds, which may affect the quality of the impregnation.

  19. Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

    PubMed

    Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

    2013-12-01

    A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results.

  20. Role of a binary metallic modifier in the determination of cadmium in graphite furnace atomic absorption spectrometry.

    PubMed

    Morimoto, Syun; Ashino, Tetsuya; Wagatsuma, Kazuaki

    2010-01-01

    In order to discuss the matrix modifier effect of palladium, iron, and a mixture of palladium and iron for the determination of cadmium in graphite-furnace atomic absorption spectrometry (GF-AAS), we measured the absorption profiles of a cadmium line at various compositions of these elements. Variations in the gas temperature were also estimated with the progress of atomization, by using a two-line method under the assumption of a Boltzmann distribution. The atomic absorption of cadmium appeared on the way of heating from the charring temperature to the atomizing temperature while the gas temperature was still low; it was thus considered that cadmium was atomized through direct conductive heating from the wall of the graphite furnace. Therefore, the effectiveness of modifiers for cadmium would be determined through any reactions on the furnace wall at the programmed charring and atomizing temperatures. The addition of iron, palladium, and an iron-palladium mixture all enhanced the absorption signal of cadmium compared to a pure cadmium sample; however, their effects were different from one another. Each addition of iron or palladium to the sample solution led to an enhancement of the cadmium absorbance, indicating that iron or palladium individually became an effective matrix modifier for the determination of cadmium. However, the addition of palladium was ineffective for the matrix modification in the coexistence of large amounts of iron. Although these phenomena are very complicated, and thus cannot be understood completely, any metallurgical reaction between the constituent elements during heating of the furnace wall, such as the formation of solid solutions and intermetallic compounds, would cause the effect of a matrix modifier in GF-AAS.

  1. Differential absorption lidar measurements of atmospheric temperature and pressure profiles

    NASA Technical Reports Server (NTRS)

    Korb, C. L.

    1981-01-01

    The theory and methodology of using differential absorption lidar techniques for the remote measurement of atmospheric pressure profiles, surface pressure, and temperature profiles from ground, air, and space-based platforms are presented. Pressure measurements are effected by means of high resolution measurement of absorption at the edges of the oxygen A band lines where absorption is pressure dependent due to collisional line broadening. Temperature is assessed using measurements of the absorption at the center of the oxygen A band line originating from a quantum state with high ground state energy. The population of the state is temperature dependent, allowing determination of the temperature through the Boltzmann term. The results of simulations of the techniques using Voigt profile and variational analysis are reported for ground-based, airborne, and Shuttle-based systems. Accuracies in the 0.5-1.0 K and 0.1-0.3% range are projected.

  2. The environmental effects of trace elements concentration in sea snails using atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    El-Amri, F. A.

    2003-05-01

    Water pollution bas increased in heavy industrialised areas. Most industrial water wastes end up in the sea. Monitoring the elemental composition in marine organisms, such as snails, provides the essential elements in living organisms and through the food chain to man. 50 samples of each of two kinds of snails have been collected from the west coast of Libya. Samples were digeste with nitric acid and the concentration of Copper, Iron, Magnesium and Zinc were determined by atomic absorption spectrometry. The results shows that Mg has the highest value while the Copper has the lowest in both kind of snaiis. A pattern of the trace elements concentration was investigated regarding the size and kind of snails.

  3. Determination of some heavy metals by flame atomic absorption spectrometry before coprecipitation with neodymium hydroxide.

    PubMed

    Soylak, Mustafa; Kizil, Nebiye

    2011-01-01

    A procedure is described for the determination of trace amounts of Cd(II), Ni(II), Cu(II), Pb(II), Fe(III), Co(II), and Mn(II) that combines flame atomic absorption spectrometry with neodymium hydroxide coprecipitation. The influences of analytical parameters (amount of neodymium, pH of the model solutions, etc.) that affect quantitative recoveries of the analyte ions were investigated. The effects of concomitant ions were also examined. The detection limits for analytes were found in the range of 0.2-3.3 microg/L. The validation of the presented procedure was controlled by analysis of certified reference materials (National Institute of Standards and Technology 1570a spinach leaves and TMDA 54.4 fortified lake water). The applications of the procedure were performed by the analysis of water, food, and herbal plants from Turkey.

  4. Determination of selenium in urine by hydride generation atomic absorption spectrometry.

    PubMed

    Navarro, M; Lopez, H; Lopez, M C; Perez, V

    1996-01-01

    A procedure has been developed for determination of total selenium in urine by hydride generation atomic absorption spectrometry. Mineralization was performed with a nitric acid-perchloric acid mixture on a thermostated digestion block. The method was validated by comparison with the method involving mineralization in a microwave acid digestion bomb containing nitric acid and small amounts of vanadium pentoxide. Se(VI) was reduced to Se(IV) by dissolution in 7N HCl. Sample recoveries, precision studies, and analyses of a certified reference material demonstrated the reliability and accuracy of this technique. Urine samples had selenium concentrations ranging from 4.6 to 50.3 micrograms/L. These values correspond to an average of 54.9 micrograms per person per day total ingested and bioavailable Se in the daily diet.

  5. Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

    PubMed

    de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2016-09-14

    An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included.

  6. [Determination of Cu, Zn and Fe in Huaiyao by suspension sampling-flame atomic absorption spectrometry].

    PubMed

    Wei, Wei; Qu, Ling-bo; Li, Jian-jun; Li, Yan-hong

    2002-10-01

    A new method--suspension sampling technique was applied to flame atomic absorption spectrometry and was successfully used to determine Cu, Zn, Fe in Huaiyao. Then studied the choice of suspension agent and elimination of chemical interference. The huaiyao sample was suspended in agar sol, and injected into air-acetylene flame by using standard addition method to determine Cu, Zn, Fe. Determined results were consistent with those obtained by HNO3 + H2SO4 + HClO4 method. The t-test showed that no obvious difference was found between the two methods. Displacement of HNO3 + H2SO4 + HClO4 method by suspension sampling method for the sample pretreatment is possible. This method is convenient, rapid and accurate.

  7. [Determination of inorganic elements in different parts of Sonchus oleraceus L by flame atomic absorption spectrometry].

    PubMed

    Wang, Nai-Xing; Cui, Xue-Gui; Du, Ai-Qin; Mao, Hong-Zhi

    2007-06-01

    Flame atomic absorption spectrometry with air-acetylene flame was used for the determination of inorganic metal elements in different parts ( flower, leaf, stem and root) of Sonchus oleraceus L. The contents of Ca, Mg, K, Na, Fe, Mn, Cu, Zn, Cr, Co, Ni, Pb and Cd in the flower, leaf, stem and root of Sonchus oleraceus L were compared. The order from high to low of the additive weight (microg x g(-1)) for the 13 kinds of metal elements is as follows: leaf (77 213.72) > flower (47 927.15) > stem(42 280.99) > root (28 131.18). From the experimental results it was found that there were considerable differences in the contents of the metal elements in different parts, and there were richer contents of Fe, Zn, Mn and Cu in root and flower, which are necessary to human health, than in other parts.

  8. Determination of arsenic in vegetable samples by hydride generation atomic absorption spectrometry

    SciTech Connect

    Navarro, M.; Lopez, M.C.; Lopez, H.; Sanchez, M.

    1992-11-01

    A procedure is described for the determination of arsenic in vegetable samples by hydride generation atomic absorption spectrometry. The samples are mineralized in a microwave acid digestion bomb with nitric acid in the presence of small amounts of vanadium pentoxide. The determination of arsenic is made by the standard addition method. A certified reference sample is analyzed, and the result obtained agreed well with the certified value. The detection limit (dry weight) was about 0.020 {mu}g/g. Reproducibility relative standard deviations ranged from 6.45% at 0.152 {mu}g As/g to 8.31% at 0.059 {mu}g As/g. The concentrations of arsenic in vegetable samples ranged from 0.029 to 0.444 {mu}g/g (fresh weight). 24 refs., 4 tabs.

  9. Determination of lead in fish samples by slurry sampling electrothermal atomic absorption spectrometry.

    PubMed

    Huang, S J; Jiang, S J

    2000-08-01

    Ultrasonic slurry sampling electrothermal atomic absorption spectrometry (USS-ETAAS) was been applied to the determination of lead in several fish samples. The influences of instrument operating conditions and slurry preparation on the signal were examined. Palladium and ammonium nitrate were used as the modifier to improve the signal. Since the sensitivity to lead in various fish slurries and aqueous solutions was different, the standard additions method was used for the determination of lead in these fish samples. The method was applied to the determination of lead in dogfish muscle reference material (DORM-2) and a swordfish muscle sample purchased from the local market. The analysis results agreed with the reference value. The accuracy was better than 6%. The precision between sample replicates was better than 16% with the USS-ETAAS method. The detection limit of lead estimated from standard additions curve was about 0.053-0.058 microgram g-1 in different samples.

  10. Quantitative analysis for a color-change of humidity indicator by microscopic absorption spectrometry.

    PubMed

    Matsumoto, Tomoko; Mitsumura, Yoko; Miyamoto, Miyuki; Matsumoto, Jin; Shiragami, Tsutomu; Fueda, Yoshiyuki; Nobuhara, Kazunori; Yasuda, Masahide

    2011-01-01

    A sensitive and easily distinguishable cobalt-free humidity indicator of porphyrin-silica gel-MgCl(2) composite was prepared from pH-induced spectra changeable tetraarylporphyrin, silica gel (SiO(2)), and MgCl(2). The pH change arose from proton release under dry conditions, and proton capture under humid conditions by a reversible reaction between MgCl(2) and a silanol group of SiO(2). A pink-orange porphyrin-Si(OH)(2)-MgCl(2) composite was dried to give a green protonated porphyrin-SiO(2)Mg composite. The optimized concentrations of MgCl(2) to make the concentrations of protonated porphyrin maximum under dry conditions were determined by absorption spectrometry of the green composite using a confocal laser scanning microscope as a microscopic spectrometer. Moreover, the green composite was prepared by heating dichloro(tetraarylporphyrinato)phosphorus chloride with MgCl(2) and SiO(2). The humidity-sensitivity of the green composite was evaluated by the absorption spectra under controlled humidity. A distinguishable color change of the green composite took place below 30% of relative humidity.

  11. Solution and slurry sampling electrothermal atomic absorption spectrometry for the analysis of high purity quartz

    NASA Astrophysics Data System (ADS)

    Hauptkorn, Susanne; Krivan, Viliam

    1996-07-01

    A slurry sampling electrothermal atomic absorption spectrometry (ETAAS) method for the determination of Al, Cr, Cu, Fe, K, Li, Mg, Mn and Na at trace and ultratrace level in high purity quartz samples has been developed. The influence of atomization temperature, internal gas flow during atomization and carbide modification of the graphite tube on the background absorption has been studied. Simple quantification via calibration curves, recorded with aqueous standards, is possible for all elements except Al. The performance and the accuracy of the slurry sampling technique are compared to those of the analysis of hydrofluoric acid digests. With both methods, the blanks could be substantially reduced by minimization of sample handling. Because of essentially higher applicable sample portions, the solution technique provides lower limits of detection for all elements excluding Al, Na and K. For the slurry sampling technique, the achievable limits of detection are in the range of 2 (Mg) to 500 (Fe) ng g -1 and for the solution technique, they are between 0.4 (Mg) and 500 (Al) ng g -1. Thus, both developed methods are well suited for ultratrace analysis of high purity quartz for microelectronic applications. The results obtained by these two ETAAS techniques are compared with those of independent methods including neutron activation analysis.

  12. Measurement of uranium series radionuclides in rock and groundwater at the Koongarra ore deposit, Australia, by gamma spectrometry

    SciTech Connect

    Yanase, Nobuyuki; Sekine, Keiichi

    1995-12-31

    Gamma spectrometry without any self-absorption correction was developed to measure low energy gamma rays emitted by uranium and actinium series radionuclides in rock samples and groundwater residues collected at the Koongarra ore deposit, Australia. Thin samples were prepared to minimize the self-absorption by uranium in the samples. The present method gave standard deviations of 0.9 to 18% for the measurements of concentrations of uranium and actinium series radionuclides. The concentrations of {sup 238}U, {sup 230}Th and {sup 235}U measured by gamma spectrometry were compared with those by alpha spectrometry that requires a complicated chemical separation procedure. The results obtained by both methods were in fairly good agreement, and it was found that the gamma spectrometry is applicable to rock and groundwater samples having uranium content sup to 8.1% (10{sup 3} B1/g) and 3 Bq/l of {sup 238}U, respectively. The detection limits were calculated to be of the order of 10{sup {minus}2} Bq/g for rock samples and 10{sup {minus}1} Bq/l for groundwater samples. The concentrations of uranium and actinium series radionuclides can be determined precisely in these samples using gamma spectrometry without any self-absorption correction.

  13. Determination of mercury in an assortment of dietary supplements using an inexpensive combustion atomic absorption spectrometry technique.

    PubMed

    Levine, Keith E; Levine, Michael A; Weber, Frank X; Hu, Ye; Perlmutter, Jason; Grohse, Peter M

    2005-01-01

    The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a result, manufacturers and regulatory agencies concerned with monitoring lot-to-lot product quality may find this approach an attractive alternative to the more classical acid-decomposition, cold vapor atomic absorption methodology. Dietary supplement samples analyzed included astragalus, calcium, chromium picolinate, echinacea, ephedra, fish oil, ginger, ginkgo biloba, ginseng, goldenseal, guggul, senna, St John's wort, and yohimbe products. Quality control samples analyzed with the dietary supplements indicated a high level of method accuracy and precision. Ten replicate preparations of a standard reference material (NIST 1573a, tomato leaves) were analyzed, and the average mercury recovery was 109% (2.0% RSD). The method quantitation limit was 0.3 ng, which corresponded to 1.5 ng/g sample. The highest found mercury concentration (123 ng/g) was measured in a concentrated salmon oil sample. When taken as directed by an adult, this product would result in an approximate mercury ingestion of 7 mug per week.

  14. Determination of Mercury in an Assortment of Dietary Supplements Using an Inexpensive Combustion Atomic Absorption Spectrometry Technique

    PubMed Central

    Levine, Michael A.; Weber, Frank X.; Hu, Ye; Perlmutter, Jason; Grohse, Peter M.

    2005-01-01

    The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a result, manufacturers and regulatory agencies concerned with monitoring lot-to-lot product quality may find this approach an attractive alternative to the more classical acid-decomposition, cold vapor atomic absorption methodology. Dietary supplement samples analyzed included astragalus, calcium, chromium picolinate, echinacea, ephedra, fish oil, ginger, ginkgo biloba, ginseng, goldenseal, guggul, senna, St John's wort, and yohimbe products. Quality control samples analyzed with the dietary supplements indicated a high level of method accuracy and precision. Ten replicate preparations of a standard reference material (NIST 1573a, tomato leaves) were analyzed, and the average mercury recovery was 109% (2.0% RSD). The method quantitation limit was 0.3 ng, which corresponded to 1.5 ng/g sample. The highest found mercury concentration (123 ng/g) was measured in a concentrated salmon oil sample. When taken as directed by an adult, this product would result in an approximate mercury ingestion of 7 μg per week. PMID:18924735

  15. Mercury speciation in hair by headspace injection-gas chromatography-atomic fluorescence spectrometry (methylmercury) and combustion-atomic absorption spectrometry (total Hg).

    PubMed

    Gao, Y; De Galan, S; De Brauwere, A; Baeyens, W; Leermakers, M

    2010-10-15

    The speciation of Hg in human hair was carried out with combustion-atomic absorption spectrometry for total Hg (THg) and headspace-gas chromatography-atomic fluorescence spectrometry (HS-GC-AFS) for methylmercury (MMHg). The determination of total Hg in hair was carried out with the AMA analyzer (Advanced Mercury Analyser 254). Accuracy and reproducibility were assessed on a Certified Reference hair sample (IAEA-086 CRM), yielding, respectively, a recovery of 97.5% and a RSD of 3.2%. Analyses of 10 blank measurements resulted in a detection limit of 1.5 ng g(-1) of THg for a 20mg sample of human hair. MMHg concentrations in hair were assessed with HS-GC-AFS in a single analysis step. Either acid or alkaline extraction can be applied because they yielded very similar results on a IAEA-086 CRM: we observed a recovery of 103% and a RSD of 7% with acid extraction and a recovery of 110% and a RSD of 9% with alkaline extraction. Optimization of the headspace vial, injection and GC parameters is described. The detection limit of the MMHg determination in human hair, which amounts to 0.04 ng g(-1) for a 20mg sample, is far below the concentrations observed in natural samples. The number of samples that can be analyzed per hour, respectively, amounts to 8 for THg and 4 for MMHg. Finally, Hg speciation in natural human hair samples was carried out by combining both AMA and HS-GC-AFS analysis methods. THg levels were at the μg g(-1), level, with an average MMHg fraction of about 70%.

  16. Application of thermospray flame furnace atomic absorption spectrometry for investigation of silver nanoparticles.

    PubMed

    Sirirat, Natnicha; Tetbuntad, Kornrawee; Siripinyanond, Atitaya

    2017-03-01

    Thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was applied to investigate the time-dependent absorption peak profile of various forms of silver. The thermospray flame furnace was set up with a 10-cm-long nickel tube with six holes, each 2.0 mm in diameter, to allow the flame to enter, and this nickel tube acted as a furnace. A sample of 300 μL was introduced into this furnace by use of water as a carrier at a flow rate of 0.5 mL min(-1) through the ceramic capillary (0.5-mm inner diameter and 2.0-mm outer diameter), which was inserted into the front hole of the nickel tube. The system was applied to examine atomization behaviors of silver nanoparticles (AgNPs) with particle sizes ranging from 10 to 100 nm. The atomization rate of AgNPs was faster than that of the dissolved silver ion. With increased amount of silver, the decay time observed from the time-dependent absorption peak profile was shortened in the case of dissolved silver ion, but it was increased in the case of AgNPs. With the particle size ranging from 10 to 100 nm, the detection sensitivity was indirectly proportional to the particle size, suggesting that TS-FF-AAS may offer insights into the particle size of AgNPs provided that the concentration of the silver is known. To obtain quantitative information on AgNPs, acid dissolution of the particles was performed before TS-FF-AAS analysis, and recoveries of 80-110% were obtained.

  17. Models of filter-based particle light absorption measurements

    NASA Astrophysics Data System (ADS)

    Hamasha, Khadeejeh M.

    Light absorption by aerosol is very important in the visible, near UN, and near I.R region of the electromagnetic spectrum. Aerosol particles in the atmosphere have a great influence on the flux of solar energy, and also impact health in a negative sense when they are breathed into lungs. Aerosol absorption measurements are usually performed by filter-based methods that are derived from the change in light transmission through a filter where particles have been deposited. These methods suffer from interference between light-absorbing and light-scattering aerosol components. The Aethalometer is the most commonly used filter-based instrument for aerosol light absorption measurement. This dissertation describes new understanding of aerosol light absorption obtained by the filter method. The theory uses a multiple scattering model for the combination of filter and particle optics. The theory is evaluated using Aethalometer data from laboratory and ambient measurements in comparison with photoacoustic measurements of aerosol light absorption. Two models were developed to calculate aerosol light absorption coefficients from the Aethalometer data, and were compared to the in-situ aerosol light absorption coefficients. The first is an approximate model and the second is a "full" model. In the approximate model two extreme cases of aerosol optics were used to develop a model-based calibration scheme for the 7-wavelength Aethalometer. These cases include those of very strong scattering aerosols (Ammonium sulfate sample) and very absorbing aerosols (kerosene soot sample). The exponential behavior of light absorption in the strong multiple scattering limit is shown to be the square root of the total absorption optical depth rather than linear with optical depth as is commonly assumed with Beer's law. 2-stream radiative transfer theory was used to develop the full model to calculate the aerosol light absorption coefficients from the Aethalometer data. This comprehensive model

  18. Inferring surface solar absorption from broadband satellite measurements

    NASA Technical Reports Server (NTRS)

    Cess, Robert D.; Vulis, Inna L.

    1989-01-01

    An atmospheric solar radiation model and surface albedo models that include wavelength dependence and surface anisotropy are combined to study the possibility of inferring the surface solar absorption from satellite measurements. The model includes ocean, desert, pasture land, savannah, and bog surface categories. Problems associated with converting narrowband measurements to broadband quantities are discussed, suggesting that it would be easier to infer surface solar absorption from broadband measurements directly. The practice of adopting a linear relationship between planetary and surface albedo to estimate surface albedos from satellite measurements is examined, showing that the linear conversion between broadband planetary and surface albedos is strongly dependent on vegetation type. It is suggested that there is a linear slope-offset relationship between surface and surface-atmosphere solar absorption.

  19. Ozone absorption cross section measurements in the Wulf bands

    NASA Technical Reports Server (NTRS)

    Anderson, Stuart M.; Hupalo, Peter; Mauersberger, Konrad

    1993-01-01

    A tandem dual-beam spectrometer has been developed to determine ozone absorption cross sections for 13 selected wavelengths between 750 and 975 nm at room temperature. The increasingly pronounced structure in this region may interfere with atmospheric trace gas transitions that are useful for remote sensing and complicate the measurement of aerosols. Ozone concentrations were determined by absorption at the common HeNe laser transition near 632.8 nm using the absolute cross section reported previously. The overall accuracy of these room temperature measurements is generally better than 2 percent. A synoptic near-IR spectrum scaled to these measurements is employed for comparison with results of previous studies.

  20. Atmospheric Water Vapour Differential Absorption Measurements with an Infrared Sounder.

    DTIC Science & Technology

    1982-03-01

    such as amonia . As the differential absorption was only of the order of 2 dB for the above measurements (at 450 m range), the measurements were repeated...frequent(ref.7), and most seriously affect surface based radio frequency sensors and communications systems. Further development and refinement of the

  1. Arsenic in marine tissues — The challenging problems to electrothermal and hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Karadjova, Irina B.; Petrov, Panayot K.; Serafimovski, Ivan; Stafilov, Trajče; Tsalev, Dimiter L.

    2007-03-01

    Analytical problems in determination of arsenic in marine tissues are addressed. Procedures for the determination of total As in solubilized or extracted tissues with tetramethylammonium hydroxide and methanol have been elaborated. Several typical lyophilized tissues were used: NIST SRM 1566a 'Oyster Tissue', BCR-60 CRM 'Trace Elements in an Aquatic Plant ( Lagarosiphon major)', BCR-627 'Forms of As in Tuna Fish Tissue', IAEA-140/TM 'Sea Plant Homogenate', NRCC DOLT-1 'Dogfish Liver' and two representatives of the Black Sea biota, Mediterranean mussel ( Mytilus galloprovincialis) and Brown algae ( Cystoseira barbata). Tissues (nominal 0.3 g) were extracted in tetramethylammonium hydroxide (TMAH) 1 ml of 25% m/v TMAH and 2 ml of water) or 5 ml of aqueous 80% v/v methanol (MeOH) in closed vessels in a microwave oven at 50 °C for 30 min. Arsenic in solubilized or extracted tissues was determined by electrothermal atomic absorption spectrometry (ETAAS) after appropriate dilution (nominally to 25 ml, with further dilution as required) under optimal instrumental parameters (pyrolysis temperature 900 °C and atomization temperature 2100 °C) with 1.5 μg Pd as modifier on Zr-Ir treated platform. Platforms have been pre-treated with 2.7 μmol of zirconium and then with 0.10 μmol of iridium which served as a permanent chemical modifier in direct ETAAS measurements and as an efficient hydride sequestration medium in flow injection hydride generation (FI-HG)-ETAAS. TMAH and methanol extract 96-108% and 51-100% of As from CRMs. Various calibration approaches have been considered and critically evaluated. The effect of species-dependent slope of calibration graph or standard additions plot for total As determination in a sample comprising of several individual As species with different ETAAS behavior has been considered as a kind of 'intrinsic element speciation interference' that cannot be completely overcome by standard additions technique. Calibration by means of CRMs has

  2. Determination of mercury in phosphate fertilizers by cold vapor atomic absorption spectrometry.

    PubMed

    de Jesus, Robson M; Silva, Laiana O B; Castro, Jacira T; de Azevedo Neto, Andre D; de Jesus, Raildo M; Ferreira, Sergio L C

    2013-03-15

    In this paper, a method for the determination of mercury in phosphate fertilizers using slurry sampling and cold vapor atomic absorption spectrometry (CV QT AAS) is proposed. Because mercury (II) ions form strong complexes with phosphor compounds, the formation of metallic mercury vapor requires the presence of lanthanum chloride as a release agent. Thiourea increases the amount of mercury that is extracted from the solid sample to the liquid phase of the slurry. The method is established using two steps. First, the slurry is prepared using the sample, lanthanum chloride, hydrochloric acid solution and thiourea solution and is sonicated for 20 min. Afterward, mercury vapor is generated using an aliquot of the slurry in the presence of the hydrochloric acid solution and isoamylic alcohol with sodium tetrahydroborate solution as the reducing agent. The experimental conditions for slurry preparation were optimized using two-level full factorial design involving the factors: thiourea and lanthanum chloride concentrations and the duration of sonication. The method allows the determination of mercury by external calibration using aqueous standards with limits of detection and quantification of 2.4 and 8.2 μg kg(-1), respectively, and precision, expressed as relative standard deviation, of 6.36 and 5.81% for two phosphate fertilizer samples with mercury concentrations of 0.24 and 0.57 mg kg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of phosphate fertilizer that was provided by the National Institute of Standards & Technology (NIST). The method was applied to determine mercury in six commercial samples of phosphate fertilizers. The mercury content varied from 33.97 to 209.28 μg kg(-1). These samples were also analyzed employing inductively coupled plasma mass spectrometry (ICP-MS). The ICP-MS results were consistent with the results from our proposed method.

  3. Measurements of scattering and absorption in mammalian cell suspensions

    SciTech Connect

    Mourant, J.R.; Johnson, T.M.; Freyer, J.P.

    1996-03-01

    During the past several years a range of spectroscopies, including fluorescence and elastic-scatter spectroscopy, have been investigated for optically based detection of cancer and other tissue pathologies. Both elastic-scatter and fluorescence signals depend, in part, on scattering and absorption properties of the cells in the tissue. Therefore an understanding of the scattering and absorption properties of cells is a necessary prerequisite for understanding and developing these techniques. Cell suspensions provide a simple model with which to begin studying the absorption and scattering properties of cells. In this study we have made preliminary measurements of the scattering and absorption properties of suspensions of mouse mammary carcinoma cells (EMT6) over a broad wavelength range (380 nm to 800 nm).

  4. Integrating Sphere Microscopy for Direct Absorption Measurements of Single Nanostructures

    PubMed Central

    2017-01-01

    Nanoscale materials are promising for optoelectronic devices because their physical dimensions are on the order of the wavelength of light. This leads to a variety of complex optical phenomena that, for instance, enhance absorption and emission. However, quantifying the performance of these nanoscale devices frequently requires measuring absolute absorption at the nanoscale, and remarkably, there is no general method capable of doing so directly. Here, we present such a method based on an integrating sphere but modified to achieve submicron spatial resolution. We explore the limits of this technique by using it to measure spatial and spectral absorptance profiles on a wide variety of nanoscale systems, including different combinations of weakly and strongly absorbing and scattering nanomaterials (Si and GaAs nanowires, Au nanoparticles). This measurement technique provides quantitative information about local optical properties that are crucial for improving any optoelectronic device with nanoscale dimensions or nanoscale surface texturing. PMID:28056171

  5. Integrating Sphere Microscopy for Direct Absorption Measurements of Single Nanostructures.

    PubMed

    Mann, Sander A; Sciacca, Beniamino; Zhang, Yunyan; Wang, Jia; Kontoleta, Evgenia; Liu, Huiyun; Garnett, Erik C

    2017-02-28

    Nanoscale materials are promising for optoelectronic devices because their physical dimensions are on the order of the wavelength of light. This leads to a variety of complex optical phenomena that, for instance, enhance absorption and emission. However, quantifying the performance of these nanoscale devices frequently requires measuring absolute absorption at the nanoscale, and remarkably, there is no general method capable of doing so directly. Here, we present such a method based on an integrating sphere but modified to achieve submicron spatial resolution. We explore the limits of this technique by using it to measure spatial and spectral absorptance profiles on a wide variety of nanoscale systems, including different combinations of weakly and strongly absorbing and scattering nanomaterials (Si and GaAs nanowires, Au nanoparticles). This measurement technique provides quantitative information about local optical properties that are crucial for improving any optoelectronic device with nanoscale dimensions or nanoscale surface texturing.

  6. Atomic Absorption Spectrometry Analysis of Trace Elements in Degenerated Intervertebral Disc Tissue

    PubMed Central

    Kubaszewski, Łukasz; Zioła-Frankowska, Anetta; Frankowski, Marcin; Nowakowski, Andrzej; Czabak-Garbacz, Róża; Kaczmarczyk, Jacek; Gasik, Robert

    2014-01-01

    Background Few studies have investigated trace elements (TE) in human intervertebral disc (IVD) tissue. Trace element presence can have diverse meanings: essential TE show the metabolic modalities of the tissue, while environmentally-related TE indicate pollution and tissue-specific absorption and accumulation. IVD is a highly specific compartment with impaired communication with adjacent bone. Analysis of TE in IVD provides new insights regarding tissue metabolism and IVD communication with other tissues. Material/Methods Thirty intervertebral discs were acquired from 22 patients during surgical treatment for degenerative disease. Atomic absorption spectrometry was used to evaluate the concentrations of Al, Cd, Pb, Cu, Ni, Mo, Mg, and Zn. Results Al, Pb, Cu, Mg, and Zn were detected in all samples. Pb was significantly positively correlated with age, and Ni concentration was weakly correlated with population count in the patient’s place of residence. Only Cu was observed in higher concentrations in IVD compared to in other tissues. Significant positive correlations were observed between the following pairs: Mg/Zn, Mg/Al, Mg/Pb, Zn/Al, Zn/Pb, and Al/Pb. Negative correlations were observed between Mg/Cd, Zn/Cd, Mg/Mo, and Mo/Pb. Conclusions This study is one of few to profile the elements in intervertebral discs in patients with degenerative changes. We report significant differences between trace element concentrations in intervertebral discs compared to in other tissues. Knowledge of the TE accumulation pattern is vital for better understanding intervertebral disc nutrition and metabolism. PMID:25366266

  7. Determination of mercury in carbon black by cold vapor atomic absorption spectrometry.

    PubMed

    Hepp, Nancy M

    2006-01-01

    Recently, a new color additive, D&C Black No. 2, a high-purity furnace black in the general category of carbon blacks, was listed as a color subject to batch certification by the U.S. Food and Drug Administration. A simple procedure was developed to determine mercury (Hg) in D&C Black No. 2, which is limited by specification to not more than 1 ppm Hg. The method uses partial acid digestion followed by cold vapor atomic absorption and was developed by modifying a method used for other color additives. The carbon black samples are treated with a mixture of nitric and hydrochloric acids and heated by microwave in sealed Teflon vessels. The resulting solutions, which are stable to Hg loss for at least 1 week, are diluted and analyzed for Hg using cold vapor atomic absorption spectrometry. Validation was performed by spiking carbon black samples with inorganic Hg (HgNO3) at levels from 0.1 to 1.5 microg/g, and by analyzing 2 standard reference materials. At the specification level of 1 ppm Hg (1 microg Hg/g), the 95% confidence interval was +/-0.01 ppm Hg (0.01 microg Hg/g). The method developed in this study gave good results for very difficult-to-analyze materials, such as coal standard reference materials and carbon black. By eliminating volatility and adsorption factors through the formation of HgCl4(-2) complexes, one can avoid using extremely hazardous acids such as HF and HClO4.

  8. Plasma absorption evidence via chirped pulse spectral transmission measurements

    SciTech Connect

    Jedrkiewicz, Ottavia; Minardi, Stefano; Couairon, Arnaud; Jukna, Vytautas; Selva, Marco; Di Trapani, Paolo

    2015-06-08

    This work aims at highlighting the plasma generation dynamics and absorption when a Bessel beam propagates in glass. We developed a simple diagnostics allowing us to retrieve clear indications of the formation of the plasma in the material, thanks to transmission measurements in the angular and wavelength domains. This technique featured by the use of a single chirped pulse having the role of pump and probe simultaneously leads to results showing the plasma nonlinear absorption effect on the trailing part of the pulse, thanks to the spectral-temporal correspondence in the measured signal, which is also confirmed by numerical simulations.

  9. Pulsed Airborne Lidar Measurements of C02 Column Absorption

    NASA Technical Reports Server (NTRS)

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

    2011-01-01

    We report on airborne lidar measurements of atmospheric CO2 column density for an approach being developed as a candidate for NASA's ASCENDS mission. It uses a pulsed dual-wavelength lidar measurement based on the integrated path differential absorption (IPDA) technique. We demonstrated the approach using the CO2 measurement from aircraft in July and August 2009 over four locations. The results show clear CO2 line shape and absorption signals, which follow the expected changes with aircraft altitude from 3 to 13 km. The 2009 measurements have been analyzed in detail and the results show approx.1 ppm random errors for 8-10 km altitudes and approx.30 sec averaging times. Airborne measurements were also made in 2010 with stronger signals and initial analysis shows approx. 0.3 ppm random errors for 80 sec averaging times for measurements at altitudes> 6 km.

  10. Effects of Solution Physical Properties on Copper and Chromium Signals in Flame Atomic Absorption Spectrometry

    NASA Astrophysics Data System (ADS)

    Rocha, Fàbio R. P.; Nòbrega, Joaquim A.

    1996-10-01

    Instrumental techniques, such as flame atomic absorption spectrometry (FAAS), are frequently used in chemical analysis. Independently of the technique used, the chemical principles must be considered to assure that the analytical results are correct. In FAAS, the most critical step is the sample introduction, since solutions need to be converted in an aerosol (nebulization process) that should contain drops with suitable size to attain the flame. Solution physical properties, such as viscosity and surface tension, can severely affect the analytical signals. Solutions with high viscosity are less easily aspirated and the analyte mass that reach the flame is reduced. The surface tension of the solution affects the size of the drops generated by the nebulization process and can modify the quantity of analyte that attain the flame. This work describes an experiment that allow demonstrating the effects of viscosity and surface tension on analytical signals, using a set of copper solutions prepared in different concentrations of ethanol and chromium solutions prepared in surfactant (tetrapropylammonium bromide) medium. The experiment can be carried out in a 4 h laboratory class and is useful to demonstrate to undergraduate students the effects of samples physical properties on the analytical signals in FAAS.

  11. Determination of trace impurities in titanium dioxide by slurry sampling electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Dong, Huang Mao; Krivan, Viliam; Welz, Bernhard; Schlemmer, Gerhard

    1997-10-01

    A slurry sampling electrothermal atomic absorption spectrometry method for the determination of Al, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Sr, Tl and Zn in powdered titanium dioxide is described. The behaviour of the titanium matrix in the atomizer and its interferences with the determination of Al, Fe, Co, Ni and Mn were studied. A tungsten carbide modified graphite tube was used to improve the signal shape and the repeatability for the determination of Fe. For all elements, except for Cd and Pb, quantification by a calibration curve established with aqueous standards was possible. No chemical modifier was used throughout in order to minimize contamination. For the contamination risk elements such as Ca, Fe, K, Mg, Na and Zn, the slurry sampling technique allows to achieve limits of detection (3 σ of the blank) 5-20 times lower than the solution technique, resulting for these elements in values of 1, 3, 0.5, 0.5, 0.9 and 2 ng g -1, respectively, and, generally being in the range of 0.2 ng g -1 (Cd) to 10 ng g -1 (Al and Tl). The results obtained by the slurry sampling technique are compared with those of other independent methods including four solution methods and neutron activation analysis.

  12. Monitoring of trace elements in honey from the Republic of Macedonia by atomic absorption spectrometry.

    PubMed

    Stankovska, Elena; Stafilov, Trajce; Sajn, Robert

    2008-07-01

    Contents of Zn, Cu, Fe, Mn, Cd, Na, K, Ca and Mg in 123 honey samples from different regions of the Republic of Macedonia were determined by atomic absorption spectrometry. A microwave digestion system was applied for digestion of the samples. The mean content for the elements determined was found to be: 2.252, 0.696, 1.885, 1.752, 0.004, 29.52, 984.8, 40.11, 18.24 mg kg(-1) for Zn, Cu, Fe, Mn, Cd, Na, K, Ca and Mg, respectively. Based on a comparison of statistical parameters, the spatial distribution of particular elements in Macedonian honey and the results of factor analysis, two natural and one anthropogenic geochemical associations were identified. The natural geochemical associations (Mg, Mn, Ca, K and Fe, Zn, Ca, -K, -Na) are influenced mainly by lithology. The anthropogenic associations (Cd and -Cu) are mostly a result of metallurgical activities, namely lead production in the town of Veles.

  13. Determination of total magnesium in biological samples using electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hulanicki, Adam; Godlewska, Beata; Brzóska, Malgorzata

    1995-11-01

    Magnesium content is an important diagnostic parameter in medicine. It is recognized that its determination in one compartment is not sufficient for reliable information about the magnesium status in the body. In addition to the common procedures of magnesium determination in blood by flame atomic absorption spectrometry, the procedure of electrothermal atomization has also been developed and applied to the analysis of blood fractions, mononuclear cells and isolated nuclei of liver cells. Electrothermal atomization is preferred in cases where the sample size is limited and the magnesium content low. The total errors are in the order of 3-4%. Various techniques of sample pretreatment have been tested and direct dilution with 0.05 mol l -1 nitric acid was optimal when the samples were not mineralized. The calibration graph based on standards containing albumin was found to give the best results, as the form of magnesium in the samples may influence the ashing and atomization processes. Good agreement was obtained for determination of magnesium in standard serum. The results are compared with those obtained by the standard flame atomization technique.

  14. [Determination of rubidium and cesium in chloride type oilfield water by flame atomic absorption spectrometry].

    PubMed

    Ye, Xiu-Shen; Zhang, Shan-Ying; Li, Hai-Jun; Li, Wu; Wu, Zhi-Jian

    2009-03-01

    Flame atomic absorption spectrometry (FAAS) was applied to the determination of rubidium and cesium in chloride type oilfield water by considering the interferences of the coexistent K+, Na+, Ca2+, and Mg2+ ions, Standard curve method and standard addition method were compared in the determination of rubidium and cesium in the simulated oilfield water and the real oilfield water from the Nanyishan region in Qaidam Basin. Although rubidium and cesium have similar physical-chemical properties, they present different characters during their analyses using the FAAS technique. When the standard addition method was used for the determination of rubidium and cesium in the simulated oilfield water, the results of rubidium were very poor, whereas the results of cesium were satisfactory. When the standard curve method was used for the determination of rubidium and cesium in the simulated oilfield water, the results of both rubidium and cesium were satisfactory within the linear ranges of the standard curves. For the real oilfield water, standard addition method is also only applicable for the determination of cesium with a recovery ranging from 90% to 110%. While standard curve method is applicable for the determination of both rubidium and cesium with a recovery ranging from 90% to 110%.

  15. Determination of Mo and V in multiphase gasoline emulsions by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Santana Sodré dos Santos, Denilson; Paixão Teixeira, Alete; das Graças Andrade Korn, Maria; Sena Gomes Teixeira, Leonardo

    2006-05-01

    This paper proposes an alternative analytical method using electrothermal atomic absorption spectrometry to determine Mo and V in multiphase gasoline emulsions. Samples were prepared by mixing gasoline with a nitric acid solution (0.1% v/v) and two cationic surfactants. The mixture was sonicated, resulting in an emulsive system. Calibration was done by using the aforementioned solutions with added analyte. The detection limits (3 σ) of Mo and V were 0.9 μg l - 1 and 4.7 μg l - 1 , respectively. The accuracy and precision of the proposed method were evaluated by the analysis of samples spiked with metallo-organic standard and the relative standard deviation obtained ranged from 1.2% to 4.4% in samples spiked with 2 μg l - 1 of each metal. The recovery rates varied from 91.2% to 101.6%. The proposed method was applied to determine Mo and V in samples of gasoline from different gas stations.

  16. Arsenic speciation in natural water samples by coprecipitation-hydride generation atomic absorption spectrometry combination.

    PubMed

    Tuzen, Mustafa; Citak, Demirhan; Mendil, Durali; Soylak, Mustafa

    2009-04-15

    A speciation procedure for As(III) and As(V) ions in environmental samples has been presented. As(V) was quantitatively recovered on aluminum hydroxide precipitate. After oxidation of As(III) by using dilute KMnO(4), the developed coprecipitation was applied to determination of total arsenic. Arsenic(III) was calculated as the difference between the total arsenic content and As(V) content. The determination of arsenic levels was performed by hydride generation atomic absorption spectrometry (HG-AAS). The analytical conditions for the quantitative recoveries of As(V) including pH, amount of aluminum as carrier element and sample volume, etc. on the presented coprecipitation system were investigated. The effects of some alkaline, earth alkaline, metal ions and also some anions were also examined. Preconcentration factor was calculated as 25. The detection limits (LOD) based on three times sigma of the blank (N: 21) for As(V) was 0.012 microg L(-1). The satisfactory results for the analysis of arsenic in NIST SRM 2711 Montana soil and LGC 6010 Hard drinking water certified reference materials for the validation of the method was obtained. The presented procedure was successfully applied to real samples including natural waters for arsenic speciation.

  17. Stabilizing Agents for Calibration in the Determination of Mercury Using Solid Sampling Electrothermal Atomic Absorption Spectrometry

    PubMed Central

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef

    2012-01-01

    Tetramethylene dithiocarbamate (TMDTC), diethyldithiocarbamate (DEDTC), and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS). These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK) extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L−1 TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants. PMID:22654606

  18. Determination of lead in fine particulates by slurry sampling electrothermal atomic absorption spectrometry.

    PubMed

    Yu, J C; Ho, K F; Lee, S C

    2001-01-02

    A simple method for determining lead in fine particulates (PM2.5) by using electrothermal atomic absorption spectrometry (ETAAS) has been developed. Particulates collected on Nuclepore filter by using a dichotomous sampler were suspended in diluted nitric acid after ultrasonic agitation. The dislodging efficiency is nearly 100% after agitation for 5 min. In order to study the suspension behavior of PM2.5 in solvents, a Brookhaven ZetaPlus Particle Size Analyzer was used to determine the particle size distribution and suspension behavior of air particulates in the solvent. The pre-digestion and modification effect of nitric acid would be discussed. Palladium was added as a chemical modifier and the temperature program of ETAAS was changed in order to improve the recovery. The slurry was introduced directly into a graphite tube for atomization. The metal content in the sample was determined by the standard addition method. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling method. It offers a quick and efficient alternative method for heavy metal characterization in fine particulates.

  19. Determination of tellurium in indium antimonide semiconductor material by electrothermal atomic absorption spectrometry.

    PubMed

    Shiue, M Y; Sun, Y C; Yang, M H

    2001-08-01

    A method for the determination of the dopant concentration of tellurium in dissolved indium antimonide semiconductor material by electrothermal atomic absorption spectrometry (ETAAS) was developed. Efforts were made to investigate the optimal conditions of the furnace heating program and the effect of palladium modifier on the variation of tellurium and the background absorbance. According to the results obtained, the presence of palladium chemical modifier in the analysis of indium antimonide allowed the successful retention of tellurium in the graphite tube, and the optimum mass of palladium modifier was found to be dependent on the sample matrix concentration. The absorbance profile of tellurium and the background level were significantly improved when a pyrolysis temperature of 1100 degrees C and an atomization temperature of 2200 degrees C were employed in the optimized heating program. With the use of this method, a detection limit of 0.8 microg g(-1) tellurium in indium antimonide could be achieved. The applicability of the proposed method was evaluated by comparison with two independent methods, i.e. slurry sampling-ETAAS and ICP-MS. From the good agreement between the results, it was demonstrated that the proposed method is suitable for the determination of typical dopant concentrations of tellurium in indium antimonide.

  20. Handling complex effects in slurry-sampling-electrothermal atomic absorption spectrometry by multivariate calibration.

    PubMed

    Felipe-Sotelo, M; Cal-Prieto, M J; Gómez-Carracedo, M P; Andrade, J M; Carlosena, A; Prada, D

    2006-07-07

    Analysis of solid samples by slurry-sampling-electrothermal atomic absorption spectrometry (SS-ETAAS) can imply spectral and chemical interferences caused by the large amount of concomitants introduced into the graphite furnace. Sometimes they cannot be solved using stabilized temperature platform furnace (STPF) conditions or typical approaches (previous sample ashing, use of chemical modifiers, etc.), which are time consuming and quite expensive. A new approach to handle interferences using multivariate calibrations (partial least squares, PLS, and artificial neural networks, ANN) is presented and exemplified with a real problem consisting on determining Sb in several solid matrices (soils, sediments and coal fly ash) as slurries by ETAAS. Experimental designs were implemented at different levels of Sb to develop the calibration matrix and assess which concomitants (seven ions were considered) modified the atomic signal mostly. They were Na+ and Ca2+ and they induced simultaneous displacement, depletion (enhancement) and broadening of the atomic peak. Here it is shown that these complex effects can be handled in a reliable, fast and cost-effective way to predict the concentration of Sb in slurry samples of several solid matrices. The method was validated predicting the concentrations of five certified reference materials (CRMs) and studying its robustness to current ETAAS problems. It is also shown that linear PLS can handle eventual non-linearities and that its results are comparable to more complex (non-linear) models, as those from ANNs.

  1. Determination of arsenic in a nickel alloy by flow injection hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hanna, C. P.; Tyson, J. F.; Offley, S. G.

    1992-08-01

    The development of a method for the direct determination of trace arsenic quantities in nickel alloy digests, by flow injection hydride generation atomic absorption spectrometry, is described. An optimization study of the manifold and chemical parameters produced system performance, in terms of tolerance of the nickel matrix and sensitivity, such that matrix removal and pre-reduction of As(V) to As (III) prior to arsine generation were eliminated. Full recovery of the As(V) signal from a solution containing 5 ng ml -1 in the presence of 60 μg ml -1 nickel was obtained. Validation of the method was achieved by analyzing a British Chemical Standard (BCS) Certified Reference Material (CRM) #346 IN nickel alloy containing arsenic at a concentration of 50 μg g -1. Following dissolution in nitric and hydrofluoric acids by a microwave assisted procedure, the only subsequent preparation required was dilution by the appropriate factor. Up to 60 injections h -1 may be made, with a detection limit of 0.5 ng ml -1 arsenic (250 pg absolute) as As(V) in a 500 μl sample. The peak height characteristic concentration is 0.46 ng ml -1, with a relative standard deviation of 3.5% for a 10 ng ml -1 As(V) standard ( n = 6).

  2. Determination of nickel in active pharmaceutical ingredients by electrothermal atomic absorption spectrometry.

    PubMed

    Bubnič, Zoran; Urleb, Uroš; Kreft, Katjuša; Veber, Marjan

    2010-03-01

    An electrothermal atomic absorption spectrometric procedure for the determination of nickel in active pharmaceutical ingredients was developed. Since the recoveries of nickel by the direct dissolution of samples in diluted nitric acid were low and caused errors in the determination of Ni in pharmaceutical samples, different approaches for sample pre-treatment were examined. It was found that the microwave digestion was the most suitable way for sample preparation. Various combinations of digestion agents and different microwave conditions were tested. The combination of nitric acid and hydrogen peroxide was found to be the most appropriate. The validity of the method was evaluated by recovery studies of spiked samples and by the comparison of the results obtained by inductively coupled plasma mass spectrometry (ICP-MS). The recovery ranged from 87.5 to 104.0% and a good agreement was achieved between both methods. The detection limit and the limit of quantification were 0.6 and 2.1 µg g-1 respectively. The precision of the method was confirmed by the determination of Ni in the spiked samples and was below 4%, expressed in terms of a relative standard deviation. The method was applied to the determination of nickel in production samples of active pharmaceutical ingredients and intermediates.

  3. Determination of mercury distribution inside spent compact fluorescent lamps by atomic absorption spectrometry.

    PubMed

    Rey-Raap, Natalia; Gallardo, Antonio

    2012-05-01

    In this study, spent compact fluorescent lamps were characterized to determine the distribution of mercury. The procedure used in this research allowed mercury to be extracted in the vapor phase, from the phosphor powder, and the glass matrix. Mercury concentration in the three phases was determined by the method known as cold vapor atomic absorption spectrometry. Median values obtained in the study showed that a compact fluorescent lamp contained 24.52±0.4ppb of mercury in the vapor phase, 204.16±8.9ppb of mercury in the phosphor powder, and 18.74±0.5ppb of mercury in the glass matrix. There are differences in mercury concentration between the lamps since the year of manufacture or the hours of operation affect both mercury content and its distribution. The 85.76% of the mercury introduced into a compact fluorescent lamp becomes a component of the phosphor powder, while more than 13.66% is diffused through the glass matrix. By washing and eliminating all phosphor powder attached to the glass surface it is possible to classified the glass as a non-hazardous waste.

  4. Investigation on binding of nitric oxide to horseradish peroxidase by absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Qiang, Li; Zhu, Shuhua; Ma, Hongmei; Zhou, Jie

    2010-01-01

    Binding of nitric oxide to horseradish peroxidase (HRP) has been investigated by absorption spectrometry in 0.2 M anaerobic phosphate buffer solution (pH 7.4). Based on this binding equilibrium, a model equation for evaluating the binding constant of nitric oxide to HRP is developed and the binding constant is calculated to be (1.55 ± 0.06) × 10 4 M -1, indicating that HRP can form a stable complex with nitric oxide. The type of inhibition by nitric oxide is validated on the basis of studying initial reaction rates of HRP-catalyzed oxidation of guaiacol in the presence of hydrogen peroxide and nitric oxide. The inhibition mechanism is found to follow an apparent non-competitive inhibition by Lineweaver-Burk method. Based on this kinetic mechanism, the binding constant is also calculated to be (5.22 ± 0.06) × 10 4 M -1. The values of the binding constant determined by the two methods are almost identical. The non-competitive inhibition model is also applicable to studying the effect of nitric oxide on other metalloenzymes, which catalyze the two-substrate reaction with the "ping-pong" mechanism.

  5. Comparison of selenium determination in liver samples by atomic absorption spectroscopy and inductively coupled plasma-mass spectrometry.

    PubMed

    Miksa, Irina Rudik; Buckley, Carol L; Carpenter, Nancy P; Poppenga, Robert H

    2005-07-01

    Selenium (Se) is an essential trace element that is often deficient in the natural diets of domestic animal species. The measurement of Se in whole blood or liver is the most accurate way to assess Se status for diagnostic purposes. This study was conducted to compare hydride generation atomic absorption spectroscopy (HG-AAS) with inductively coupled plasma-mass spectrometry (ICP-MS) for the detection and quantification of Se in liver samples. Sample digestion was accomplished with magnesium nitrate and nitric acid for HG-AAS and ICP-MS, respectively. The ICP-MS detection was optimized for 82Se with yttrium used as the internal standard and resulted in a method detection limit of 0.12 microg/g. Selenium was quantified by both methods in 310 samples from a variety of species that were submitted to the Toxicology Laboratory at New Bolton Center (Kennett Square, PA) for routine diagnostic testing. Paired measurements for each sample were evaluated by a mean difference plot method. Limits of agreement were used to describe the maximum differences likely to occur between the 2 methods. Results suggest that under the specified conditions ICP-MS can be reliably used in place of AAS for quantitation of tissue Se at or below 2 microg/g to differentiate between adequate and deficient liver Se concentrations.

  6. Automated on-line preconcentration of trace aqueous mercury with gold trap focusing for cold vapor atomic absorption spectrometry.

    PubMed

    Puanngam, Mahitti; Dasgupta, Purnendu K; Unob, Fuangfa

    2012-09-15

    A fully automated system for the determination of trace mercury in water by cold vapor atomic absorption spectrometry (CVAAS) is reported. The system uses preconcentration on a novel sorbent followed by liberation of the mercury and focusing by a gold trap. Mercury ions were extracted from water samples by passage through a solid phase sorbent column containing 2-(3-(2-aminoethylthio)propylthio)ethanamine modified silica gel. The captured mercury is released by thiourea and then elemental Hg is liberated by sodium borohydride. The vapor phase Hg is recaptured on a gold-plated tungsten filament. This is liberated as a sharp pulse (half-width<2 s) by directly electrically heating the tungsten filament in a dry argon stream. The mercury is measured by CVAAS; no moisture removal is needed. The effects of chloride and selected interfering ions were studied. The sample loading flow rate and argon flow rates for solution purging and filament sweeping were optimized. An overall 50-fold improvement in the limit of detection was observed relative to direct measurement by CVAAS. With a relatively modest multi-user instrument we attained a limit of detection of 35 ng L(-1) with 12% RSD at 0.20 μg L(-1) Hg level. The method was successfully applied to accurately determine sub-μg L(-1) level Hg in standard reference water samples.

  7. Alpha spectrometry — A tool for nuclear data measurements

    NASA Astrophysics Data System (ADS)

    Wiltshire, R. A. P.

    1984-06-01

    Alpha spectrometry is a precise technique which can be applied to the measurement of data such as half-lives and the production cross-sections of higher actinides. The application of this technique to the measurement of 239Pu and 242Cm half-lives, to the production cross-sections for curium isotopes in fast reactor spectra and to the analysis of irradiated fuel for alpha emitting higher actinide nuclides are discussed.

  8. Automation of long-path absorption cell measurements.

    PubMed

    Watkins, W R; Dixon, R G

    1979-01-01

    Recent advances have been made in the operation of long-path absorption cells which make them easier to align and improve the accuracy of measurements made with them. Only one person is required now for routine measurements of low absorption coefficients of atmospheric absorbers. Unique gear designs for the adjustment of the cell mirrors are described which utilize low-torque linear drives and make possible rapid changes in pathlength and precision repositioning of the cell output beam at long pathlengths. Automation of cell operation by the use of remote Selsyn controls is described. Several techniques are discussed for precision optical alignment of long-path absorption cells, including the use of infrared radiation sources. The system accuracy which results from these refinements in operation is included.

  9. Tone-burst technique measures high-intensity sound absorption

    NASA Technical Reports Server (NTRS)

    Powell, J. G.; Van Houten, J. J.

    1971-01-01

    Tone-burst technique, in which narrow-bandwidth, short-duration sonic pulse is propagated down a standing-wave tube, measures sound absorbing capacity of materials used in jet engine noise abatement. Technique eliminates effects of tube losses and yields normal-incidence absorption coefficient of specimen.

  10. Measurement of incidence angle dependence of solar absorptance

    NASA Astrophysics Data System (ADS)

    Ohnishi, A.; Hayashi, T.

    1983-12-01

    For measuring solar absorptance dependence on incidence angle, an integrating sphere, in which the sample is fixed on the surface of the sphere, and the incident angle for the monochromatic beam on the surface is adjusted by the rotation of the integrating sphere, is proposed. Results for spacecraft materials are presented. Results for aluminized Teflon are 4% better compared with the standard method.

  11. Recent improvements in PDS technique for low-absorption measurements

    NASA Astrophysics Data System (ADS)

    Montecchi, Marco; Masetti, Enrico; Emiliani, Gabriele

    1990-08-01

    Photothermal Deflection Spectroscopy (PDS) is a recently developed technique that is finding a useful application in the measurement of low optical absorptance of thin films. Among the noise sources affecting the PDS measurement, probe beam pointing instability and mechanical vibration play a considerable role. In this work an optoelectronic system for the reduction of their influence is described. Moreover, PDS measurements are typically performed keeping the sample immersed in a deflecting liquid; thus measured values of absorptance must be corrected when other surrounding media, as air, are considered. This correction is an easy task for single film coatings. Here the general case of an unknown multiplayer coating is analysed; a range of values containing the true absorptance in air is obtained by theoretical analysis and a practical method to evaluate the absorptance in air is discussed. Finally, deflecting liquids alternative to the commonly used CCI4 have been examined. Useful optical range, thermal diffusivity and "relative deflecting power" of CCI4, CS2, Iso-octane and Aceton are reported.

  12. Multi-element analysis of manganese nodules by atomic absorption spectrometry without chemical separation

    USGS Publications Warehouse

    Kane, J.S.; Harnly, J.M.

    1982-01-01

    Five manganese nodules, including the USGS reference nodules A-1 and P-1, were analyzed for Co, Cu, Fe, K, Mg, Mn, Na, Ni and Zn without prior chemical separation by using a simultaneous multi-element atomic absorption spectrometer with an air-cetylene flame. The nodules were prepared in three digestion matrices. One of these solutions was measured using sixteen different combinations of burner height and air/acetylene ratios. Results for A-1 and P-1 are compared to recommended values and results for all nodules are compared to those obtained with an inductively coupled plasma. The elements Co, Cu, Fe, K, Mg, Mn, Na, Ni, and Zn are simultaneously determined with a composite recovery for all elements of 100 ?? 7%, independent of the digestion matrices, heights in the flame, or flame stoichiometries examined. Individual recoveries for Co, K, and Ni are considerably poorer in two digests than this composite figure, however. The optimum individual recoveries of 100 ?? 5% and imprecisions of 1-4%, except for zinc, are obtained when Co, K, Mn, Na and Ni are determined simultaneously in a concentrated digest, and in another analytical sequence, when Cu, Fe, Mg, Mn and Zn are measured simultaneously after dilution. Determination of manganese is equally accurate in the two sequences; its measurement in both assures internal consistency between the two measurement sequences. This approach improves analytical efficiency over that for conventional atomic absorption methods, while minimizing loss of accuracy or precision for individual elements. ?? 1982.

  13. Sample pre-treatment methods for the trace elements determination in seafood products by atomic absorption spectrometry.

    PubMed

    Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Adela

    2002-07-03

    Different sample pre-treatments for seafood products have been compared with determine trace elements (As, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Se and Zn) by flame atomic absorption spectrometry (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). Classic pre-treatments as microwave assisted-acid digestion and the slurry sampling technique were compared with new procedures such as microwave energy or ultrasound energy assisted-acid leaching process and enzymatic hydrolysis methodologies based on the use of pronase E. The methods were applied to DORM-1 and DOLT-1 reference materials with certified contents for the studied elements. The Student-Newman-Keuls (SNK) method was used to compare with element concentration means obtained with each sample pre-treatment and also the certified concentration means in both reference materials. Multivariate techniques such as principal components analysis (PCA) was also applied to comparative purposes.

  14. Determination of sulfur in bovine serum albumin and L-cysteine using high-resolution continuum source molecular absorption spectrometry of the CS molecule

    NASA Astrophysics Data System (ADS)

    Andrade-Carpente, Eva; Peña-Vázquez, Elena; Bermejo-Barrera, Pilar

    2016-08-01

    In this study, the content of sulfur in bovine serum albumin and L-cysteine was determined using high-resolution continuum source molecular absorption spectrometry of the CS molecule, generated in a reducing air-acetylene flame. Flame conditions (height above the burner, measurement time) were optimized using a 3.0% (v/v) sulfuric acid solution. A microwave lab station (Ethos Plus MW) was used for the digestion of both compounds. During the digestion step, sulfur was converted to sulfate previous to the determination. Good repeatability (4-10%) and analytical recovery (91-106%) was obtained.

  15. Measurements of scattering and absorption changes in muscle and brain.

    PubMed Central

    Gratton, E; Fantini, S; Franceschini, M A; Gratton, G; Fabiani, M

    1997-01-01

    Non-invasive techniques for the study of human brain function based on changes of the haemoglobin content or on changes of haemoglobin saturation have recently been proposed. Among the new methods, near-infrared transmission measurements may have significant advantages and complement well-established methods such as functional magnetic resonance imaging and positron emission tomography. Near-infrared measurements can be very fast, comparable in speed to electrophysiological measurements, bur are better localized. We will present the demonstration of measurements of millisecond signals due to brain activity in humans following stimulation of the visual cortex. However, major unresolved questions remain about the origin of the signals observed. Optical measurements on exposed cortex in animals show that both the absorption and the scattering coefficient are affected by neural activity. Model calculations show that the signals we detected may originate from rapid changes of the scattering coefficient in a region about 1 to 2 cm below the scalp. We discuss our measurement protocol, which is based on a frequency-domain instrument, and the algorithm to separate the absorption from the scattering contribution in the overall response. Our method produces excellent separation between scattering and absorption in relatively homogeneous masses such as large muscles. The extrapolation of our measurement protocol to a complex structure such as the human head is critically evaluated. PMID:9232861

  16. Absorption of sound in air - High-frequency measurements

    NASA Technical Reports Server (NTRS)

    Bass, H. E.; Shields, F. D.

    1977-01-01

    The absorption of sound in air at frequencies from 4 to 100 kHz in 1/12 octave intervals, for temperatures from 255.4 K (0 F) to 310.9 K (100 F) in 5.5 K (10 F) intervals, and at 10% relative-humidity increments between 0% and saturation has been measured. The values of free-field absorption have been analyzed to determine the relaxation frequency of oxygen for each of the 92 combinations of temperature and relative humidity studied and the results are compared to an empirical expression. The relaxation frequencies of oxygen have been analyzed to determine the microscopic energy-transfer rates.

  17. Robotized sampling device for graphite furnace atomic absorption spectrometry slurry analysis with Varian SpectrAA instruments

    NASA Astrophysics Data System (ADS)

    Hoenig, Michel; Cilissen, Anne

    1993-08-01

    There is a growing interest in the determination by electrothermal atomic absorption spectrometry (ETAAS) of elements in solid samples without a dissolution stage, to avoid contamination and losses during the preparation of the sample. This approach may be particularly convenient when only small amounts of sample are available. Details of the above-mentioned program for the adaptation of the Gilson sample changer to Varian SpectrAA systems (X,Y,Z positions, timings etc.) are available on request.

  18. Determination of cadmium in biodiesel using microemulsion and electrothermal atomization atomic absorption spectrometry.

    PubMed

    Lima, Adriana S; Silva, Deise G; Teixeira, Leonardo S G

    2015-01-01

    This work aimed to prepare biodiesel microemulsions for the subsequent quantification of cadmium via graphite furnace atomic absorption spectrometry (GFAAS). The biodiesel samples were prepared using n-propanol as an emulsifier, 10% (v/v) nitric acid as the aqueous phase, and biodiesel. Pseudoternary phase diagrams were constructed to determine the microemulsion region with the specified components. The optimized conditions for microemulsion formation were 57.6% (v/v) n-propanol, 21.2% (v/v) biodiesel, and 21.2% (v/v) nitric acid solution. The stability of the microemulsified system was investigated using aqueous and organic standards, and the system was found to be stable for at least 240 min. The applied pyrolysis and atomization temperatures were 800 and 2000 °C, respectively, and 5 μg of aluminum was used as the chemical modifier. The obtained limits of detection and quantification were 0.2 and 0.5 μg kg(-1), respectively, and the characteristic mass was 1.6 pg. The precision, expressed as the relative standard deviation (% R.S.D., n = 10), was 2.5% for a sample with a cadmium concentration of 6.5 μg kg(-1). The accuracy was determined from addition and recovery experiments, with results varying from 93 to 108% recovery. This study demonstrates that the proposed method based on the use of a microemulsion formation in sample preparation can be applied as an efficient alternative for the determination of cadmium in biodiesel by GFAAS. Cadmium determination in biodiesel samples of different origins (soybean, corn, cotton, and sunflower) was evaluated after acid digestion using the inductively coupled plasma-mass spectrometry (ICP-MS) technique, and the obtained results were compared to the results obtained using the proposed method. The paired t test (95% confidence level) did not show significant differences. The concentrations of cadmium found ranged from 5.3 to 8.0 μg kg(-1).

  19. Prediction of absorption coefficients by pulsed laser induced photoacoustic measurements.

    PubMed

    Priya, Mallika; Satish Rao, B S; Ray, Satadru; Mahato, K K

    2014-06-05

    In the current study, a pulsed laser induced photoacoustic spectroscopy setup was designed and developed, aiming its application in clinical diagnostics. The setup was optimized with carbon black samples in water and with various tryptophan concentrations at 281nm excitations. The sensitivity of the setup was estimated by determining minimum detectable concentration of tryptophan in water at the same excitation, and was found to be 0.035mM. The photoacoustic experiments were also performed with various tryptophan concentrations at 281nm excitation for predicting optical absorption coefficients in them and for comparing the outcomes with the spectrophotometrically-determined absorption coefficients for the same samples. Absorption coefficients for a few serum samples, obtained from some healthy female volunteers, were also determined through photoacoustic and spectrophotometric measurements at the same excitations, which showed good agreement between them, indicating its clinical implications.

  20. Towards higher stability of resonant absorption measurements in pulsed plasmas

    SciTech Connect

    Britun, Nikolay; Michiels, Matthieu; Snyders, Rony

    2015-12-15

    Possible ways to increase the reliability of time-resolved particle density measurements in pulsed gaseous discharges using resonant absorption spectroscopy are proposed. A special synchronization, called “dynamic source triggering,” between a gated detector and two pulsed discharges, one representing the discharge of interest and another being used as a reference source, is developed. An internal digital delay generator in the intensified charge coupled device camera, used at the same time as a detector, is utilized for this purpose. According to the proposed scheme, the light pulses from the reference source follow the gates of detector, passing through the discharge of interest only when necessary. This allows for the utilization of short-pulse plasmas as reference sources, which is critical for time-resolved absorption analysis of strongly emitting pulsed discharges. In addition to dynamic source triggering, the reliability of absorption measurements can be further increased using simultaneous detection of spectra relevant for absorption method, which is also demonstrated in this work. The proposed methods are illustrated by the time-resolved measurements of the metal atom density in a high-power impulse magnetron sputtering (HiPIMS) discharge, using either a hollow cathode lamp or another HiPIMS discharge as a pulsed reference source.

  1. Low-frequency sound absorption measurements in air

    NASA Technical Reports Server (NTRS)

    Zuckerwar, A. J.; Meredith, R. W.

    1984-01-01

    Thirty sets of sound absorption measurements in air at a pressure of 1 atmosphere are presented at temperatures from 10 C to 50 C, relative humidities from 0 to 100 percent, and frequencies from 10 to 2500 Hz. The measurements were conducted by the method of free decay in a resonant tube having a length of 18.261 m and bore diameter of 0.152 m. Background measurements in a gas consisting of 89.5 percent N2 and 10.5 percent Ar, a mixture which has the same sound velocity as air, permitted the wall and structural losses of the tube to be separated from the constituent absorption, consisting of classical rotational and vibrational absorption, in the air samples. The data were used to evaluate the vibrational relaxation frequencies of N2 and/or O2 for each of the 30 sets of meteorological parameters. Over the full range of humidity, the measured relaxation frequencies of N2 in air lie between those specified by ANSI Standard S1.26-1978 and those measured earlier in binary N2H2O mixtures. The measured relaxation frequencies could be determined only at very low values of humidity, reveal a significant trend away from the ANSI standard, in agreement with a prior investigation.

  2. Evaluation of arsenic, cobalt, copper and manganese in biological Samples of Steel mill workers by electrothermal atomic absorption Spectrometry.

    PubMed

    Afridi, H I; Kazi, T G; Kazi, N G; Jamali, M K; Arain, M B; Sirajuddin; Kandhro, G A; Shah, A Q; Baig, J A

    2009-02-01

    The determination of trace and toxic elements in biological samples (blood, urine and scalp hair samples) of human beings is an important clinical test. The aim of our present study was to determine the concentration of arsenic (As), copper (Cu), cobalt (Co) and manganese (Mn), in biological samples of male production workers (PW) and quality control workers (QW) of steel mill, with aged 25-55 years, to assess the possible influence of environmental exposure. For comparison purpose, the same biological samples of unexposed healthy males of same age group were collected as control subjects. The determination of all elements in biological samples was carried out by electrothermal atomic absorption spectrometry, prior to microwave assisted acid digestion. The accuracy of the As, Cu, Co and Mn measurements was tested by simultaneously analyzing certified reference materials (CRMs) and for comparative purposes conventional wet acid digestion method was used on the same CRMs. No significant differences were observed between the analytical results and the certified values, using both methods (paired t-test at P > 0.05). The results indicate that concentrations of As, Cu, Co and Mn in all three biological samples of the exposed workers (QW and PW) were significantly higher than those of the controls. The possible correlation of these elements with the etiology of different physiological disorders is discussed. The results were also demonstrated the need of attention for improvements in workplace, ventilation and industrial hygiene practices.

  3. Tellurium speciation analysis using hydride generation in situ trapping electrothermal atomic absorption spectrometry and ruthenium or palladium modified graphite tubes.

    PubMed

    Yildirim, Emrah; Akay, Pınar; Arslan, Yasin; Bakirdere, Sezgin; Ataman, O Yavuz

    2012-12-15

    Speciation of tellurium can be achieved by making use of different kinetic behaviors of Te(IV) and Te(VI) upon their reaction with sodium borohydride using hydride generation. While Te(IV) can form H(2)Te, Te(VI) will not form any volatile species during the course of hydride formation and measurement by atomic absorption spectrometry. Quantitative reduction of Te(VI) was achieved through application of a microwave assisted prereduction of Te(VI) in 6.0 mol/L HCl solution. Enhanced sensitivity was achieved by in situ trapping of the generated H(2)Te species in a previously heated graphite furnace whose surface was modified using Pd or Ru. Overall efficiency for in situ trapping in pyrolytically coated graphite tube surface was found to be 15% when volatile analyte species are trapped for 60s at 300°C. LOD and LOQ values were calculated as 0.086 ng/mL and 0.29 ng/mL, respectively. Efficiency was increased to 46% and 36% when Pd and Ru surface modifiers were used, respectively. With Ru modified graphite tube 173-fold enhancement was obtained over 180 s trapping period with respect to ETAAS; the tubes could be used for 250 cycles. LOD values were 0.0064 and 0.0022 ng/mL for Pd and Ru treated ETAAS systems, respectively, for 180 s collection of 9.6 mL sample solution.

  4. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A.

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v- 1 of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L- 1 with a limit of detection of 4.9 μg L- 1 and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L- 1 Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials.

  5. Determination of aluminium and manganese in human scalp hair by electrothermal atomic absorption spectrometry using slurry sampling.

    PubMed

    Bermejo-Barrera, P; Moreda-Piñeiro, A; Moreda-Piñeiro, J; Bermejo-Barrera, A

    1998-04-01

    Methods for the determination of aluminium and manganese in human scalp hair samples by electrothermal atomic absorption spectrometry using the slurry sampling technique were developed. Palladium and magnesium nitrate were used as chemical modifiers. Hair samples were pulverized using a zirconia vibrational mill ball, and were prepared as aqueous slurries. Determinations can be performed in the linear ranges of 1.9-150 mug l(-1) Al(3+) and 0.03-10.0 mug l(-1) Mn(2+). Limits of detection of 0.9 mg kg(-1) and 27.6 mug kg(-1) were obtained for aluminium and manganese, respectively. The analytical recoveries were between 99.6 and 101.8% for aluminium and in the 98.3-101.3% range for manganese. The repeatability of the methods (n=11), slurry preparation procedure and ETAAS measurement, was 16.0 and 7.9% for aluminium and manganese, respectively. The methods were finally applied to the aluminium and manganese determination in 25 scalp hair samples from healthy adults. The levels for aluminium were between 8.21 and 74.08 mg kg(-1), while concentrations between 0.03 and 1.20 mg kg(-1) were found for manganese.

  6. Preconcentration of gold ions from water samples by modified organo-nanoclay sorbent prior to flame atomic absorption spectrometry determination.

    PubMed

    Afzali, Daryoush; Mostafavi, Ali; Mirzaei, Mohammad

    2010-09-15

    In this work, the applicability of modified organo nanoclay as a new and easy prepared solid sorbent for the preconcentration of trace amounts of Au(III) ion from water samples is studied. The organo nanoclay was modified with 5-(4'-dimethylamino benzyliden)-rhodanine and used as a sorbent for separation of Au(III) ions. The sorption of gold ions was quantitative in the pH range of 2.0-6.0. Quantitative desorption occurred with 6.0 mL of 1.0 mol L(-1) Na(2)S(2)O(3). The amount of eluted Au(III) was measured using flame atomic absorption spectrometry. In the initial solution the linear dynamic range was in the range of 0.45 ng mL(-1) to 10.0 microg mL(-1), the detection limit was 0.1 ng mL(-1) and the preconcentration factor was 105. Also, the relative standard deviation was +/-2.3% (n=8 and C=2.0 microg mL(-1)) and the maximum capacity of the sorbent was 3.9 mg of Au(III) per gram of modified organo nanoclay. The influences of the experimental parameters including sample pH, eluent volume and eluent type, sample volume, and interference of some ions on the recoveries of the gold ion were investigated. The proposed method was applied for preconcentration and determination of gold in different samples.

  7. Nickel and strontium nitrates as modifiers for the determination of selenium in wine by Zeeman electrothermal atomic absorption spectrometry.

    PubMed

    Cvetković, J; Stafilov, T; Mihajlović, D

    2001-08-01

    A mixed matrix modifier of nickel and strontium nitrates was used as a chemical modifier for the determination of selenium in wines by Zeeman electrothermal atomic absorption spectrometry. Wine samples were heated on a boiling water bath with small amounts of nitric acid and hydrogen peroxide. For complete elimination of interference, especially from sulfates and phosphates, selenium is complexed with ammonium pyrolidinedithiocarbamate (APDTC), extracted into methyl isobutyl ketone (MIBK), and measured by ETAAS. The graphite furnace temperature program was optimized for both aqueous and organic solutions. Pyrolysis temperatures of 1300 degrees C and 800 degrees C were chosen for aqueous and organic solutions, respectively; 2700 degrees C and 2100 degrees C were used as optimum atomization temperatures for aqueous and organic solutions, respectively. The optimum modifier mass established is markedly lower than those presented in the literature. The platform atomization ensures pretreatment stabilization up to 1100 degrees C and 1600 degrees C, respectively, for organic and aqueous selenium solutions. The procedure was verified by the method of standard addition. The investigated wine samples originated from the different regions of the Republic of Macedonia. The selenium concentration varied from not detectable to 0.93 microg L(-1).

  8. Atomic Absorption Spectroscopy, Atomic Emission Spectroscopy, and Inductively Coupled Plasma-Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Miller, Dennis D.; Rutzke, Michael A.

    Atomic spectroscopy has played a major role in the development of our current database for mineral nutrients and toxicants in foods. When atomic absorption spectrometers became widely available in the 1960s, the development of atomic absorption spectroscopy (AAS) methods for accurately measuring trace amounts of mineral elements in biological samples paved the way for unprecedented advances in fields as diverse as food analysis, nutrition, biochemistry, and toxicology (1). The application of plasmas as excitation sources for atomic emission spectroscopy (AES) led to the commercial availability of instruments for inductively coupled plasma - atomic emission spectroscopy (ICP-AES) beginning in the late 1970s. This instrument has further enhanced our ability to measure the mineral composition of foods and other materials rapidly, accurately, and precisely. More recently, plasmas have been joined with mass spectrometers (MS) to form inductively coupled plasma-mass spectrometer ICP-MS instruments that are capable of measuring mineral elements with extremely low detection limits. These three instrumental methods have largely replaced traditional wet chemistry methods for mineral analysis of foods, although traditional methods for calcium, chloride, iron, and phosphorus remain in use today (see Chap. 12).

  9. Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

    USGS Publications Warehouse

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

  10. Temporal variations in gas temperature in an atomization stage of cadmium and tellurium evaluated by using the two-line method in graphite furnace atomic absorption spectrometry.

    PubMed

    Shimabukuro, Haruki; Ashino, Tetsuya; Wagatsuma, Kazuaki

    2008-09-01

    In order to discuss the atomization process of an analyte element occurring in a graphite furnace for atomic absorption spectrometry, we measured variations in the characteristic temperature with the progress of an atomization stage, by using a two-line method under the assumption of a Boltzmann distribution. For this purpose, iron was chosen as the analyte element. Also, the atomic absorption of two iron atomic lines, Fe I 372.0 nm and Fe I 373.7 nm, was simultaneously monitored as a probe for the temperature determination. This method enables variations in the gas temperature to be directly traced, yielding a temperature distribution closely related to the diffusion behavior of the probe element in the furnace. This temperature variation was very different from the furnace wall temperatures, which were monitored in conventional temperature control for atomic absorption spectrometry. Correlations between the gas temperature and the charring/atomizing temperatures in the heating program of the furnace were investigated. The atomization of cadmium and tellurium was also investigated by a comparison between the gas temperature with the wall temperature of the furnace. The atomic absorption of cadmium or tellurium appeared to be apart from the absorption of iron while the gas temperature was still low. Therefore, the analyte atoms could be atomized through direct contact with the wall of the graphite furnace, which has a much higher temperature compared to the gas atmosphere during atomization. Their atomization would be caused by conductive heating from the furnace wall rather than by radiant heating in the furnace.

  11. Absorptance Measurements of Optical Coatings - A Round Robin

    SciTech Connect

    Chow, R; Taylor, J R; Wu, Z L; Boccara, C A; Broulik, U; Commandre, M; DiJon, J; Fleig, C; Giesen, A; Fan, Z X; Kuo, P K; Lalezari, R; Moncur, K; Obramski, H-J; Reicher, D; Ristau, D; Roche, P; Steiger, B; Thomsen, M; von Gunten, M

    2000-10-26

    An international round robin study was conducted on the absorption measurement of laser-quality coatings. Sets of optically coated samples were made by a ''reactive DC magnetron'' sputtering and an ion beam sputtering deposition process. The sample set included a high reflector at 514 nm and a high reflector for the near infrared (1030 to 1318 nm), single layers of silicon dioxide, tantalum pentoxide, and hafnium dioxide. For calibration purposes, a sample metalized with hafnium and an uncoated, superpolished fused silica substrate were also included. The set was sent to laboratory groups for absorptance measurement of these coatings. Whenever possible, each group was to measure a common, central area and another area specifically assigned to the respective group. Specific test protocols were also suggested in regards to the laser exposure time, power density, and surface preparation.

  12. Ozone absorption coefficients' role in Dobson instrument ozone measurement accuracy

    NASA Astrophysics Data System (ADS)

    Basher, R. E.

    1982-11-01

    The differences of 10% or more between the laboratory measurements of UV absorption coefficients by different investigators indicate accuracies that are quite inadequate for current needs in the measurement of atmospheric ozone. The standard band-integrated set of coefficients now used with the Dobson instrument are mutually consistent to about 2%, but their absolute accuracy is still in question. The accurate calculation of band-integrated coefficients must take account of their dependence on source spectral irradiance, atmospheric spectral transmittance, mean ozone temperature, and instrument spectral transmittance. A careful examination shows that Komhyr's (1980) case for an error of about +5% in the standard Dobson AD ozone estimation is subject to large uncertainties and certain lacks of independence. The obvious solution to this accuracy problem lies in better laboratory measurements of ozone absorption.

  13. Direct analysis of reference biofluids by coupled in situ electrodeposition-electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Matousek, Jaroslav P.; Powell, Kipton J.

    1999-12-01

    The application of coupled in situ electrodeposition-electrothermal atomic absorption spectrometry (ED-ETAAS) to the determination of Pb in biological standard reference materials is described. In situ electrodeposition at a cell voltage of 3.0 V from 25-μl samples onto electrodeposited Pd is used to quantitatively separate the analyte from blood and urine matrices. With subsequent withdrawal of spent electrolyte, this overcomes the atomisation problems inherent with high salt and organic contents. ED-ETAAS is applied with minimal sample pre-treatment (acidification). The electrolysis process aids decomposition of the organic matrix, and the release of trace elements. Evolution of H 2 at the cathode counters fouling of the Pd modifier surface. The palladium deposit is renewed in situ for each determination. For AMI certified lyophilised blood, diluted 1+3 with 0.1 M HCl (18.1 μg/l Pb), the R.S.D. was 3.0% (peak height; n=5) and the detection limit (3 σ blank; n=5) was 1.5 μg/l. Results for certified blood samples were AMI 72.3±4.3 μg/l (certified 76.2±7.6 μg/l) and Seronorm 34.2±2.0 μg/l (36±4 μg/l). The result for NIST SRM 2670 normal urine acidified to 1% HNO 3 was 8.1±0.6 μg/l (recommended value 10 μg/l).

  14. [Determination of metals in Ginkgo biloba leaves by atomic absorption spectrometry with microwave digestion].

    PubMed

    Jiang, Bo; Jiang, Guo-Bin; Liu, Chang-Jian; Ma, Kun; Jin, Li-Ming; Gao, Jiang-Mei

    2010-03-01

    Microwave digestion technique was used in the decomposition of Ginkgo biloba leaves from six different trees at the same age in the same area. HNO3-H2O2 (5 : 1 v/v) was used as microwave digestion agent at a suitable temperature and time. The contents of Ca, Mg, K, Na, Cu, Zn and Zn/Cu were determined by flame atomic absorption spectrometry to study the distribution rule of metallic elements in the trees at the same age and in the same area. The recovery ratio ranged from 95.2% to 104.6%. The results showed that there were certain differences between different trees in the distribution of metallic elements. The contents of calcium were from 39 586 to 48 320 microg x g(-1), and those of magnesium from 10 076 to 12 918 microg x g(-1), of potassium from 2 004 to 5 240 microg x g(-1), of sodium from 9.05 to 35.30 microg x g(-1), and of copper from 1.50 to 3.05 microg x g(-1), while Zn/Cu values were from 2.68 to 5.93 in the leaves of 6 different trees in the same growing area. Therefore there were abounding calcium, magnesium and potassium, while the content of sodium and Zn/Cu values were lower, and the metal contents were different in the leaves. The experimental results provided useful bases for studying the distribution rule of metallic elements in Ginkgo biloba leaves, the relationship between the contents of calcium, magnesium, potassium and sodium and the Zn/Cu value in ginkgo biloba leaves and the treatment for cardio-cerebral vascular disease.

  15. Determination and interference studies of bismuth by tungsten trap hydride generation atomic absorption spectrometry.

    PubMed

    Kula, Ibrahim; Arslan, Yasin; Bakirdere, Sezgin; Titretir, Serap; Kendüzler, Erdal; Ataman, O Yavuz

    2009-11-15

    The determination of bismuth requires sufficiently sensitive procedures for detection at the microg L(-1) level or lower. W-coil was used for on-line trapping of volatile bismuth species using HGAAS (hydride generation atomic absorption spectrometry); atom trapping using a W-coil consists of three steps. Initially BiH(3) gas is formed by hydride generation procedure. The analyte species in vapor form are transported through the W-coil trap held at 289 degrees C where trapping takes place. Following the preconcentration step, the W-coil is heated to 1348 degrees C; analyte species are released and transported to flame-heated quartz atom cell where the atomic signal is formed. In our study, interferences have been investigated in detail during Bi determination by hydride generation, both with and without trap in the same HGAAS system. Interferent/analyte (mass/mass) ratio was kept at 1, 10 and 100. Experiments were designed for carrier solutions having 1.0M HNO(3). Interferents such as Fe, Mn, Zn, Ni, Cu, As, Se, Cd, Pb, Au, Na, Mg, Ca, chloride, sulfate and phosphate were examined. The calibration plot for an 8.0 mL sampling volume was linear between 0.10 microg L(-1) and 10.0 microg L(-1) of Bi. The detection limit (3s/m) was 25 ng L(-1). The enhancement factor for the characteristic concentration (C(o)) was found to be 21 when compared with the regular system without trap, by using peak height values. The validation of the procedure was performed by the analysis of the certified water reference material and the result was found to be in good agreement with the certified values at the 95% confidence level.

  16. Scattering error corrections for in situ absorption and attenuation measurements.

    PubMed

    McKee, David; Piskozub, Jacek; Brown, Ian

    2008-11-24

    Monte Carlo simulations are used to establish a weighting function that describes the collection of angular scattering for the WETLabs AC-9 reflecting tube absorption meter. The equivalent weighting function for the AC-9 attenuation sensor is found to be well approximated by a binary step function with photons scattered between zero and the collection half-width angle contributing to the scattering error and photons scattered at larger angles making zero contribution. A new scattering error correction procedure is developed that accounts for scattering collection artifacts in both absorption and attenuation measurements. The new correction method does not assume zero absorption in the near infrared (NIR), does not assume a wavelength independent scattering phase function, but does require simultaneous measurements of spectrally matched particulate backscattering. The new method is based on an iterative approach that assumes that the scattering phase function can be adequately modeled from estimates of particulate backscattering ratio and Fournier-Forand phase functions. It is applied to sets of in situ data representative of clear ocean water, moderately turbid coastal water and highly turbid coastal water. Initial results suggest significantly higher levels of attenuation and absorption than those obtained using previously published scattering error correction procedures. Scattering signals from each correction procedure have similar magnitudes but significant differences in spectral distribution are observed.

  17. Solar absorptance measurements in space on operational spacecraft

    NASA Astrophysics Data System (ADS)

    Babel, Hank W.; Jones, Cherie A.; Wilkes, Donald R.; Linton, Roger C.

    1995-07-01

    Spacecraft hardware such as radiators requires the maintenance of solar absorptance within tight bounds for their design life. Such hardware is sized in part based on the beginning- and end-of-life absorptance. It has been difficult to make accurate end-of-life determinations based on either ground based data or flight data. The synergistic effect of atomic oxygen, ultraviolet radiation, and contamination has made it difficult to duplicate space exposures in the laboratory. The absorptance of flight exposed samples brought back to earth are not representative of the conditions in space because of changes brought about by exposure to air. This paper proposes to augment the current in-space monitoring techniques with periodic, in- space, direct measurements of the solar absorptance on operational hardware. NASA funded AZ Technology to develop a portable, space-rated device similar to the LPSR-200 portable spectroreflectometer, a space portable spectroreflectometer (SPSR). This instrument is robotically compatible and can be run using spacecraft power or batteries. The instrument also has measurement storage capacity for later retrieval and evaluation. Although extensive development work has already been completed, authorization to build a unit for a flight experiment has not been received. The Russians have expressed an interest in having absorptance measurements made on their MIR I Space Station as part of the NASA/MIR flight experiments. Proposals are currently being made to obtain authorization for the construction and use of SPSR on NASA/MIR flight experiments, to help mitigate potential problems for the International Space Station Alpha (ISSA).

  18. Automated continuous monitoring of inorganic and total mercury in wastewater and other waters by flow-injection analysis and cold-vapour atomic absorption spectrometry

    PubMed Central

    Birnie, S. E.

    1988-01-01

    An automated continuous monitoring system for the determination of inorganic and total mercury by flow-injection analysis followed by cold-vapour atomic absorption spectrometry is described. The method uses a typical flow-injection manifold where digestion and reduction of the injected sample takes place. Mercury is removed by aeration from the flowing stream in a specially designed air-liquid separator and swept into a silica cell for absorption measurement at a wavelength of 253.7 nm. A calibration curve up to 10 μg Hg ml-1 using three different path length cells is obtained with a detection limit of 0.02 μg Hg ml-1. The sampling rate of an injection every 3 min produces 20 results per hour from a flowing stream. PMID:18925201

  19. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Sardans, Jordi; Montes, Fernando; Peñuelas, Josep

    2010-02-01

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at μg L -1 levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages of

  20. Speciation analysis of arsenic in biological matrices by automated hydride generation-cryotrapping-atomic absorption spectrometry with multiple microflame quartz tube atomizer (multiatomizer).

    EPA Science Inventory

    This paper describes an automated system for the oxidation state specific speciation of inorganic and methylated arsenicals by selective hydride generation - cryotrapping- gas chromatography - atomic absorption spectrometry with the multiatomizer. The corresponding arsines are ge...

  1. Cortisol production rates measured by liquid chromatography/mass spectrometry

    SciTech Connect

    Esteban, N.V.; Yergey, A.L. )

    1990-04-01

    Cortisol production rates (FPRs) in physiologic and pathologic states in humans have been investigated over the past 30 years. However, there has been conflicting evidence concerning the validity of the currently accepted value of FPRs in humans (12 to 15 mg/m2/d) as determined by radiotracer methodology. The present study reviews previous methods proposed for the measurement of FPRs in humans and discusses the applications of the first method for the direct determination of 24-hour plasma FPRs during continuous administration of a stable isotope, using a thermospray high-pressure liquid chromatography-mass spectrometry technique. The technique is fast, sensitive, and, unlike gas chromatography-mass spectrometry methods, does not require derivatization, allowing on-line detection and quantification of plasma cortisol after a simple extraction procedure. The results of determination of plasma FPRs by stable tracer/mass spectrometry are directly in units of mass/time and, unlike radiotracer methods, are independent of any determination of volume of distribution or cortisol concentration. Our methodology offers distinct advantages over radiotracer techniques in simplicity and reliability since only single measurements of isotope ratios are required. The technique was validated in adrenalectomized patients. Circadian variations in daily FRPs were observed in normal volunteers, and, to date, results suggest a lower FRP in normal children and adults than previously believed. 88 references.

  2. Excited State Absorption Measurements In Some Scintillator Dye Solutions

    NASA Astrophysics Data System (ADS)

    Dharamsi, A., N.; Jong, Shawpin; Hassam, A. B.

    1986-11-01

    Time-resolved excited state triplet-triplet absorption spectra were measured for solutions of 2,5 diphenyloxazole (PPO) and 2,1 napthyl, 5 phenyloxazole (aNPO) in several solvents. Concentration quenching effects due to excimer formation in nonaromatic solvents were observed. A numerical analysis of the experimental results yielded the rate constants for intersystem crossing, triplet quenching by 02, triplet self quenching and the formation of excimers.

  3. Direct absorption measurements in thin rods and optical fibers

    NASA Astrophysics Data System (ADS)

    Mühlig, Christian; Bublitz, Simon; Lorenz, Martin

    2015-11-01

    We report on the first realization of direct absorption measurements in thin rods and optical fibers using the laser induced deflection (LID) technique. Typically, along the fiber processing chain more or less technology steps are able to introduce additional losses to the starting material. After the final processing, the fibers are commonly characterized regarding losses using the so-called cut-back technique in combination with spectrometers. This, however, only serves for a total loss determination. For optimization of the fiber processing, it would be of great interest to not only distinguish between different loss mechanisms but also have a better understanding of possible causes. For measuring the absorption losses along the fiber processing, a particular concept for the LID technique is introduced and requirements, calibration procedure as well as first results are presented. It allows to measure thin rods, e.g. during preform manufacturing, as well as optical fibers. In addition, the results show the prospects to also apply the new concept to topics like characterizing unwanted absorption after fiber splicing or Bragg grating inscription.

  4. Determination of sodium and potassium in nanoliter volumes of biological fluids by furnace atomic absorption spectrometry

    SciTech Connect

    Nash, L.A.; Peterson, L.N.; Nadler, S.P.; Levine, D.Z.

    1988-11-01

    Renal tubular fluid samples are nanoliter (10/sup -9/ L) volumes containing sodium and potassium concentrations that are within the range of determination by furnace atomic absorption. Modification of nanoliter handling techniques and the use of microboats with the IL 951/655 provided a method for rapid precise analyses (relative standard deviation of 5%). Determinations of sodium and potassium were precise; however, inaccuracies occurred with anion substitution of sodium salts. NaHCO/sub 3/ solutions gave consistently higher peak height absorbance and area absorbance compared with those of NaCl: the peak area absorbance correlated linearly with the concentration of bicarbonate. Pretreatment of the microboat with boric acid eliminated this phenomenon and the associated inaccuracy. Comparison of determination of sodium in nanoliter samples by graphite furnace atomic absorption with macroanalysis by flame emission gave relative errors of less than 2.0%. Addition of sodium and potassium to tubular fluid samples yielded mean recoveries of 102.6% and 99.7%, respectively. The authors conclude that graphite furnace can be an accurate method for measurement of sodium and potassium in nanoliter volumes of biological fluids.

  5. Analytical Validation of Accelerator Mass Spectrometry for Pharmaceutical Development: the Measurement of Carbon-14 Isotope Ratio.

    SciTech Connect

    Keck, B D; Ognibene, T; Vogel, J S

    2010-02-05

    Accelerator mass spectrometry (AMS) is an isotope based measurement technology that utilizes carbon-14 labeled compounds in the pharmaceutical development process to measure compounds at very low concentrations, empowers microdosing as an investigational tool, and extends the utility of {sup 14}C labeled compounds to dramatically lower levels. It is a form of isotope ratio mass spectrometry that can provide either measurements of total compound equivalents or, when coupled to separation technology such as chromatography, quantitation of specific compounds. The properties of AMS as a measurement technique are investigated here, and the parameters of method validation are shown. AMS, independent of any separation technique to which it may be coupled, is shown to be accurate, linear, precise, and robust. As the sensitivity and universality of AMS is constantly being explored and expanded, this work underpins many areas of pharmaceutical development including drug metabolism as well as absorption, distribution and excretion of pharmaceutical compounds as a fundamental step in drug development. The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of {sup 14}C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the {sup 14}C label), stable across samples storage conditions for at least one year, linear over 4 orders of magnitude with an analytical range from one tenth Modern to at least 2000 Modern (instrument specific). Further, accuracy was excellent between 1 and 3 percent while precision expressed as coefficient of variation is between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of carbon-14 (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with {sup 14}C corresponds to 30 fg

  6. Rhodium as permanent modifier for atomization of lead from biological fluids using tungsten filament electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Zhou, Ying; Parsons, Patrick J.; Aldous, Kenneth M.; Brockman, Paul; Slavin, Walter

    2002-04-01

    Rhodium (Rh) was investigated as a permanent modifier for the atomization of Pb from biological fluids in W-filament atomic absorption spectrometry (AAS). Heating the W-filament with a Rh solution provided a protective coating for subsequent determinations of Pb in blood and urine matrices. The W-filament AAS instrumentation used was based on a prototype design that utilized self-reversal background correction scheme and peak area measurements. We found that Rh not only stabilized Pb during the pyrolysis step, but also facilitated the removal of carbonaceous residues during the cleaning step, requiring much less power than with phosphate modifier. Thus, the filament lifetime was greatly extended to over 300 firings. Periodic reconditioning with Rh was necessary every 30 firings or so. Conditioning the filament with Rh also permitted direct calibration using simple aqueous Pb standards. The method detection limit for blood Pb was approximately 1.5 μg dl -1, similar to that reported previously. Potential interferences from concomitants such as Na, K, Ca and Mg were evaluated. Accuracy was verified using lead reference materials from the National Institute of Standards and Technology and the New York State Department of Health. Blood lead results below 40 μg dl -1 were within ±1 μg dl -1 of certified values, and within ±10% above 40 μg dl -1; within-run precision was ±10% or better. Additional validation was reported using proficiency test materials and human blood specimens. All blood lead results were within the acceptable limits established by regulatory authorities in the US. When measuring Pb in urine, sensitivity was reduced and matrix-matched calibration became necessary. The method of detection limit was 27 μg l -1 for urine Pb. Urine lead results were also validated using an acceptable range comparable to that established for blood lead by US regulatory agencies.

  7. Evidence for aluminum-binding erythropoietin by size-exclusion chromatography coupled to electrothermal absorption atomic spectrometry.

    PubMed

    Veiga, Marlei; Bohrer, Denise; Noremberg, Simone; do Nascimento, Paulo C; de Carvalho, Leandro M

    2011-11-01

    Erythropoietin (EPO) is a glycoprotein that stimulates erythropoiesis and is clinically used for treating anemia during chronic renal failure and for anemia in preterm infants. EPO formulations usually have elevated rates of contamination due to aluminum (Al), which is toxic to both types of patients. Size-exclusion chromatography (SEC) coupled with graphite furnace atomic absorption spectrometry (GF AAS) was employed to separate proteins and to quantify the amount of aluminum present in the elution volume corresponding to EPO and, therefore, to evaluate possible binding. Because EPO formulations contain human serum albumin (HSA), a chromatographic method was optimized for the separation of these proteins. Subsequent to the chromatographic separation, 1-mL fractions of the column effluent were collected, and the Al content in these aliquots was measured by GF AAS. EPO and HSA samples were incubated with Al for 4h at 4°C and 37°C as well as for 16 h at 4°C and 37°C. Afterwards, they were injected into the chromatographic system. These samples were also submitted to ultrafiltration (10 and 50 kDa membranes), and Al was measured in the ultrafiltrates. The results showed that Al was present in the eluent volume corresponding to the EPO peak but not in the HSA peak in the chromatograms. Temperature strengthened the interaction because the Al present in the EPO fraction was 3 times higher at 37°C compared to 4°C. Thirty-eight percent of the Al present in a 2.4 μg/mL EPO standard solution, and approximately 50% of the Al in formulation samples containing approximately 11 μg/mL EPO and either citrate or phosphate, were non-ultrafiltrable, which suggests that EPO is an effective Al acceptor in vitro.

  8. Determination of thallium in wine by electrothermal atomic absorption spectrometry after extraction preconcentration

    NASA Astrophysics Data System (ADS)

    Cvetković, Julijana; Arpadjan, Sonja; Karadjova, Irina; Stafilov, Trajče

    2002-06-01

    A simple method for extraction electrothermal atomic absorption spectroscopy (ETAAS) determination of Tl in wine is described. The wine sample is decomposed with a mixture of nitric acid and hydrogen peroxide and both thallium species Tl(I) and Tl(III) are extracted from 0.5 mol l -1 KI solution into iso-butyl methyl ketone (IBMK). Optimal parameters for ETAAS measurement of the iodide complexes extracted were defined for two different instruments: Perkin Elmer Zeeman 3030 (HGA 600) and Varian SpectrAA-880 (GTA-100). Modifiers of tartaric acid, Pd [ammoniumtetrachloropaladate (II)] or Ag (silver nitrate) were investigated for thermal stabilization of such extremely volatile species as iodide complexes of Tl. The analytical procedure developed permits 50-fold preconcentration and determination of 0.05 μg l -1 Tl in wine. The relative standard deviation ranges from 6 to 12% for the concentration range 0.2-1 μg l -1 Tl in wine.

  9. Transient Infrared Measurement of Laser Absorption Properties of Porous Materials

    NASA Astrophysics Data System (ADS)

    Marynowicz, Andrzej

    2016-06-01

    The infrared thermography measurements of porous building materials have become more frequent in recent years. Many accompanying techniques for the thermal field generation have been developed, including one based on laser radiation. This work presents a simple optimization technique for estimation of the laser beam absorption for selected porous building materials, namely clinker brick and cement mortar. The transient temperature measurements were performed with the use of infrared camera during laser-induced heating-up of the samples' surfaces. As the results, the absorbed fractions of the incident laser beam together with its shape parameter are reported.

  10. Interpreting measurements obtained with the cloud absorption radiometer

    NASA Technical Reports Server (NTRS)

    1988-01-01

    The software developed for the analysis of data from the Cloud Absorption Radiometer (CAR) is discussed. The CAR is a multichannel radiometer designed to measure the radiation field in the middle of an optically thick cloud (the diffusion domain). It can also measure the surface albedo and escape function. The instrument currently flies on a C-131A aircraft operated by the University of Washington. Most of this data was collected during the First International satellite cloud climatology project Regional Experiment (FIRE) Marine Stratocumulus Intensive Field Observation program off San Diego during July 1987. Earlier flights of the CAR have also been studied.

  11. Simultaneous determination of cadmium and lead in wine by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Freschi, Gian P. G.; Dakuzaku, Carolina S.; de Moraes, Mercedes; Nóbrega, Joaquim A.; Gomes Neto, José A.

    2001-10-01

    A method has been developed for the direct simultaneous determination of Cd and Pb in white and red wine by electrothermal atomic absorption spectrometry (ET-AAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect background correction. The thermal behavior of both analytes during pyrolysis and atomization stages were investigated in 0.028 mol l -1 HNO 3 and in 1+1 v/v diluted wine using mixtures of Pd(NO 3) 2+Mg(NO 3) 2 and NH 4H 2PO 4+Mg(NO 3) 2 as chemical modifiers. With 5 μg Pd+3 μg Mg as the modifiers and a two-step pyrolysis (10 s at 400°C and 10 s at 600°C), the formation of carbonaceous residues inside the atomizer was avoided. For 20 μl of sample (wine+0.056 mol l -1 HNO 3, 1+1, v/v) dispensed into the graphite tube, analytical curves in the 0.10-1.0 μg l -1 Cd and 5.0-50 μg l -1 Pb ranges were established. The characteristic mass was approximately 0.6 pg for Cd and 33 pg for Pb, and the lifetime of the tube was approximately 400 firings. The limits of detection (LOD) based on integrated absorbance (0.03 μg l -1 for Cd, 0.8 μg l -1 for Pb) exceeded the requirements of Brazilian Food Regulations (decree #55871 from Health Department), which establish the maximum permissible level for Cd at 200 μg l -1 and for Pb at 500 μg l -1. The relative standard deviations ( n=12) were typically <8% for Cd and <6% for Pb. The recoveries of Cd and Pb added to wine samples varied from 88 to 107% and 93 to 103%, respectively. The accuracy of the direct determination of Cd and Pb was checked for 10 table wines by comparing the results with those obtained for digested wine using single-element ET-AAS, which were in agreement at the 95% confidence level.

  12. Integrated measurements of 222Rn by absorption in Makrofol

    NASA Astrophysics Data System (ADS)

    Pressyanov, Dobromir; Buysse, Jozef; Poffijn, André; Van Deynse, Annick; Meesen, Geert

    2004-01-01

    Recently, a method for long-term 222Rn measurements based on the radon absorption ability and track-etch properties of Makrofol has been proposed. The basic idea is to remove, after exposure, a surface layer, thicker than the range of the α-particles of the 222Rn or 220Rn progenies, and to study the track density of the electrochemically etched tracks at that depth. This paper summarizes the performance of the method under laboratory and field conditions. The effects on the response due to differences in pressure, temperature, humidity, the presence of 220Rn, dust and cigarette smoke in the air have been studied experimentally. The effect of these factors, but the temperature, is either absent, or restricted to about 10% for the very extreme cases. The variation of the response at the studied depth of 83 μm over the temperature interval 15-25°C is ±12% around the 19.5°C value. The field comparison conducted showed an agreement between the method of radon absorption in Makrofol and the conventional diffusion chambers. Therefore, a potential for long-term 222Rn measurements in the human environment by radon absorption in Makrofol or equivalent polycarbonates clearly exists.

  13. The Importance of Optical Pathlength Control for Plasma Absorption Measurements

    NASA Technical Reports Server (NTRS)

    Cruden, Brett A.; Rao, M. V. V. S.; Sharma, Surendra P.; Meyyappan, M.; Partridge, Harry (Technical Monitor)

    2001-01-01

    An inductively coupled GEC Cell with modified viewing ports has been used to measure in-situ absorption in CF4 plasmas via Fourier Transform Infrared Spectroscopy, and the results compared to those obtained in a standard viewport configuration. The viewing ports were modified so that the window boundary is inside, rather than outside, of the GEC cell. Because the absorption obtained is a spatially integrated absorption, measurements made represent an averaging of absorbing species inside and outside of the plasma. This modification is made to reduce this spatial averaging and thus allow a more accurate estimation of neutral species concentrations and temperatures within the plasmas. By reducing this pathlength, we find that the apparent CF4 consumption increases from 65% to 95% and the apparent vibrational temperature of CF4 rises by 50-75 K. The apparent fraction of etch product SiF4 decreases from 4% to 2%. The data suggests that these density changes may be due to significant temperature gradients between the plasma and chamber viewports.

  14. Accelerator Mass Spectrometry for Measurement of Long-Lived Radioisotopes

    NASA Astrophysics Data System (ADS)

    Elmore, David; Phillips, Fred M.

    1987-05-01

    Particle accelerators, such as those built for research in nuclear physics, can also be used together with magnetic and electrostatic mass analyzers to measure rare isotopes at very low abundance ratios. All molecular ions can be eliminated when accelerated to energies of millions of electron volts. Some atomic isobars can be eliminated with the use of negative ions; others can be separated at high energies by measuring their rate of energy loss in a detector. The long-lived radioisotopes 10Be, 14C, 26Al, 36Cl, and 129I can now be measured in small natural samples having isotopic abundances in the range 10-12 to 10-15 and as few as 105 atoms. In the past few years, research applications of accelerator mass spectrometry have been concentrated in the earth sciences (climatology, cosmochemistry, environmental chemistry, geochronology, glaciology, hydrology, igneous petrogenesis, minerals exploration, sedimentology, and volcanology), in anthropology and archeology (radiocarbon dating), and in physics (searches for exotic particles and measurement of half-lives). In addition, accelerator mass spectrometry may become an important tool for the materials and biological sciences.

  15. Accelerator mass spectrometry for measurement of long-lived radioisotopes.

    PubMed

    Elmore, D; Phillips, F M

    1987-05-01

    Particle accelerators, such as those built for research in nuclear physics, can also be used together with magnetic and electrostatic mass analyzers to measure rare isotopes at very low abundance ratios. All molecular ions can be eliminated when accelerated to energies of millions of electron volts. Some atomic isobars can be eliminated with the use of negative ions; others can be separated at high energies by measuring their rate of energy loss in a detector. The long-lived radioisotopes (10)Be, (14)C,(26)A1, 36Cl, and (129)1 can now be measured in small natural samples having isotopic abundances in the range 10(-12) to 10(- 5) and as few as 10(5) atoms. In the past few years, research applications of accelerator mass spectrometry have been concentrated in the earth sciences (climatology, cosmochemistry, environmental chemistry, geochronology, glaciology, hydrology, igneous petrogenesis, minerals exploration, sedimentology, and volcanology), in anthropology and archeology (radiocarbon dating), and in physics (searches for exotic particles and measurement of halflives). In addition, accelerator mass spectrometry may become an important tool for the materials and biological sciences.

  16. Excited-state absorption measurements of Tm3+-doped crystals

    NASA Astrophysics Data System (ADS)

    Szela, J. W.; Mackenzie, J. I.

    2012-06-01

    High resolution, absolute excited-state absorption (ESA) spectra, at room temperature, from the long-lived 3F4 energy level of several crystals doped with trivalent thulium (Tm3+) ions have been measured employing high-brightness narrowband (FWHM <30 nm) light emitting diodes (LEDs) as a probe wavelength. The aim of this investigation was to determine the strength of ESA channels at wavelengths addressable by commercially available semiconductor laser diodes operating around 630-680 nm. The favourable lifetime of the 3F4 manifold and negligible ground-state absorption (GSA) for the red-wavelength second-step excitation, ensures a direct and efficient route for a dual-wavelength pumping scheme of the thulium ion, which will enable blue-green laser emission from its 1G4 upper-laser level.

  17. Determining the Uncertainty of X-Ray Absorption Measurements

    PubMed Central

    Wojcik, Gary S.

    2004-01-01

    X-ray absorption (or more properly, x-ray attenuation) techniques have been applied to study the moisture movement in and moisture content of materials like cement paste, mortar, and wood. An increase in the number of x-ray counts with time at a location in a specimen may indicate a decrease in moisture content. The uncertainty of measurements from an x-ray absorption system, which must be known to properly interpret the data, is often assumed to be the square root of the number of counts, as in a Poisson process. No detailed studies have heretofore been conducted to determine the uncertainty of x-ray absorption measurements or the effect of averaging data on the uncertainty. In this study, the Poisson estimate was found to adequately approximate normalized root mean square errors (a measure of uncertainty) of counts for point measurements and profile measurements of water specimens. The Poisson estimate, however, was not reliable in approximating the magnitude of the uncertainty when averaging data from paste and mortar specimens. Changes in uncertainty from differing averaging procedures were well-approximated by a Poisson process. The normalized root mean square errors decreased when the x-ray source intensity, integration time, collimator size, and number of scanning repetitions increased. Uncertainties in mean paste and mortar count profiles were kept below 2 % by averaging vertical profiles at horizontal spacings of 1 mm or larger with counts per point above 4000. Maximum normalized root mean square errors did not exceed 10 % in any of the tests conducted. PMID:27366627

  18. Differential Absorption Lidar (DIAL) Measurements from Air and Space

    NASA Technical Reports Server (NTRS)

    Browell, E. V.; Ismail, S.; Grant, W. B.

    1998-01-01

    Differential absorption lidar (DIAL) systems have been used for the measurement of ozone, water vapor, and aerosols from aircraft platforms for over 18 years, yielding new insights into atmospheric chemistry, composition, and dynamics in large-scale field experiments conducted all over the world. The successful deployment of the lidar in-space technology experiment (LITE) in September 1994 demonstrated that space-based lidars can also collect valuable information on the global atmosphere. This paper reviews some of the contributions of the NASA Langley Research Center's airborne ozone and water vapor DIAL systems and space-based LITE system to the understanding of the atmosphere and discusses the feasibility and advantages of putting DIAL systems in space for routine atmospheric measurements of ozone and/or water vapor and aerosols and clouds. The technology and applications of the differential absorption lidar (DIAL) technique have progressed significantly since the first DIAL measurements of Schotland, and airborne DIAL measurements of ozone and water vapor are frequently being made in a wide range of field experiments. In addition, plans are underway to develop DIAL systems for use on satellites for continuous global measurements. This paper will highlight the history of airborne lidar and DIAL systems, summarize the major accomplishments of the NASA Langley DIAL program, and discuss specifications and goals for DIAL systems in space.

  19. Guide to plutonium isotopic measurements using gamma-ray spectrometry

    SciTech Connect

    Lemming, J.F.; Rakel, D.A.

    1982-08-26

    Purpose of this guide is to assist those responsible for plutonium isotopic measurements in the application of gamma-ray spectrometry. Objectives are to promote an understanding of the measurement process, including its limitations and applicability, by reviewing the general features of a plutonium spectrum and identifying the quantities which must be extracted from the data; to introduce state-of-the-art analysis techniques by reviewing four isotopic analysis packages and identifying their differences; to establish the basis for measurement control and assurance by discussing means of authenticating the performance of a measurement system; and to prepare for some specific problems encountered in plutonium isotopic analyses by providing solutions from the practical experiences of several laboratories. 29 references, 12 figures, 17 tables.

  20. Method development for the determination of bromine in coal using high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis

    NASA Astrophysics Data System (ADS)

    Pereira, Éderson R.; Castilho, Ivan N. B.; Welz, Bernhard; Gois, Jefferson S.; Borges, Daniel L. G.; Carasek, Eduardo; de Andrade, Jailson B.

    2014-06-01

    This work reports a simple approach for Br determination in coal using direct solid sample analysis in a graphite tube furnace and high-resolution continuum source molecular absorption spectrometry. The molecular absorbance of the calcium mono-bromide (CaBr) molecule has been measured using the rotational line at 625.315 nm. Different chemical modifiers (zirconium, ruthenium, palladium and a mixture of palladium and magnesium nitrates) have been evaluated in order to increase the sensitivity of the CaBr absorption, and Zr showed the best overall performance. The pyrolysis and vaporization temperatures were 800 °C and 2200 °C, respectively. Accuracy and precision of the method have been evaluated using certified coal reference materials (BCR 181, BCR 182, NIST 1630a, and NIST 1632b) with good agreement (between 98 and 103%) with the informed values for Br. The detection limit was around 4 ng Br, which corresponds to about 1.5 μg g- 1 Br in coal, based on a sample mass of 3 mg. In addition, the results were in agreement with those obtained using electrothermal vaporization inductively coupled plasma mass spectrometry, based on a Student t-test at a 95% confidence level. A mechanism for the formation of the CaBr molecule is proposed, which might be considered for other diatomic molecules as well.

  1. Studies of cavity enhanced absorption spectroscopy for weak absorption gas measurements

    NASA Astrophysics Data System (ADS)

    Li, Liucheng; Duo, Liping; Gong, Deyu; Ma, Yanhua; Zhang, Zhiguo; Wang, Yuanhu; Zhou, Dongjian; Jin, Yuqi

    2017-01-01

    In order to determine the concentrations of trace amount metastable species in chemical lasers, an off-axis cavity enhanced absorption spectrometer for the detection of weak absorption gases has been built with a noise equivalent absorption sensitivity of 1.6x10-8 cm-1. The absorption spectrum of trace amount gaseous ammonia and water vapor was obtained with a spectral resolution of about 78 MHz. A multiple-line absorption spectroscopic method to determine the temperature of gaseous ammonia has been developed by use of multiple lines of ammonia molecule absorption spectrum.

  2. Determination of lithium isotopes at natural abundance levels by atomic absorption spectrometry

    USGS Publications Warehouse

    Meier, A.L.

    1982-01-01

    The relationships of the absorption of 6Li and 7Li hollow cathode lamp emissions are used to determine lithium isotopic composition in the natural abundance range of geologic materials. Absorption was found to have a nonlinear dependence upon total lithium concentration and isotopic composition. A method using nonlinear equations to describe the relationship of the absorption of 6Li and 7Li lamp radiation is proposed as a means of calculating isotopic composition that is independent of total lithium concentration.

  3. La pulvérisation par ultra-sons appliquée à la spectrometrie d'absorption atomique.

    PubMed

    Spitz, J; Uny, G

    1968-07-01

    Ultrasonic nebulization applied to atomic absorption spectrometry gives a sensitivity ten to twenty times better than that which can be obtained by classical pneumatic nebulization. This gain in sensitivity is primarily due to the quantity of aerosol introduced into the flame, but is equally due to the fineness of the droplets that are formed. The study of certain parameters (frequency, power applied to the emitter, geometry of the nebulizing chamber, gas flow) has led to the specification of an ultrasonic nebulizer that can be conveniently used for routine analyses.

  4. Determination of cadmium and lead in edible oils by electrothermal atomic absorption spectrometry after reverse dispersive liquid-liquid microextraction.

    PubMed

    López-García, Ignacio; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel

    2014-06-01

    The dispersive liquid-liquid microextraction of edible oils with a low volume of an acidic solution in the presence of isopropyl alcohol allows cadmium and lead to be completely separated into the aqueous phase. After centrifugation, the metals are determined by electrothermal atomization atomic absorption spectrometry using a palladium salt for chemical modification in the heating cycle. Using a 10 g oil sample, the enrichment factor is 140, which permits detection limits of 0.6 and 10 ng kg(-1) for cadmium and lead, respectively. The results agree with those obtained after sample mineralization. Data for the cadmium and lead levels for 15 samples of different characteristics are given.

  5. Determination of the measurement threshold in gamma-ray spectrometry.

    PubMed

    Korun, M; Vodenik, B; Zorko, B

    2017-03-01

    In gamma-ray spectrometry the measurement threshold describes the lover boundary of the interval of peak areas originating in the response of the spectrometer to gamma-rays from the sample measured. In this sense it presents a generalization of the net indication corresponding to the decision threshold, which is the measurement threshold at the quantity value zero for a predetermined probability for making errors of the first kind. Measurement thresholds were determined for peaks appearing in the spectra of radon daughters (214)Pb and (214)Bi by measuring the spectrum 35 times under repeatable conditions. For the calculation of the measurement threshold the probability for detection of the peaks and the mean relative uncertainty of the peak area were used. The relative measurement thresholds, the ratios between the measurement threshold and the mean peak area uncertainty, were determined for 54 peaks where the probability for detection varied between some percent and about 95% and the relative peak area uncertainty between 30% and 80%. The relative measurement thresholds vary considerably from peak to peak, although the nominal value of the sensitivity parameter defining the sensitivity for locating peaks was equal for all peaks. At the value of the sensitivity parameter used, the peak analysis does not locate peaks corresponding to the decision threshold with the probability in excess of 50%. This implies that peaks in the spectrum may not be located, although the true value of the measurand exceeds the decision threshold.

  6. Measurement of Acoustic Attenuation and Absorption Coefficients using Thermometry

    NASA Astrophysics Data System (ADS)

    Morris, Hugh; Rivens, Ian; Shaw, Adam; ter Haar, Gail

    2007-05-01

    Accurate knowledge of both the attenuation and the absorption coefficient of tissue are required when planning an optimal high intensity focused ultrasound treatment. A novel technique for simple measurement of this parameters has been developed in which a thin-film thermocouple (TFT) is placed between two layers of tissue of different thicknesses. The sample can be rotated about an axis through the junction of the TFT so that it can be insonated from either side leaving the tissue adjacent to the junction unchanged, but changing the overlying thickness. The attenuation and absorption coefficients can be calculated from the heating curves measured in the two orientations. Experiments have been carried out in both tissue mimicking material (TMM) and in ex vivo liver tissue. Weakly focused transducers, resonant at 1.05 MHz, 2.4 MHz and 3.55 MHz were used at free-field spatial peak intensities of 9-14 W/cm2. The temperature rise was measured as a function of time using a TFT. These thermocouples are not subject to the viscous heating artefact that is common to other thermocouple devices and so are advantageous for this purpose. Alignment was achieved with a 3D automated gantry system, which was controlled with specialised software. Timing and data acquisition were also controlled with this software. All experiments were carried out in degassed water. Results for TMM and degassed excised bovine liver are presented.

  7. Measurements of parallel electron velocity distributions using whistler wave absorption

    SciTech Connect

    Thuecks, D. J.; Skiff, F.; Kletzing, C. A.

    2012-08-15

    We describe a diagnostic to measure the parallel electron velocity distribution in a magnetized plasma that is overdense ({omega}{sub pe} > {omega}{sub ce}). This technique utilizes resonant absorption of whistler waves by electrons with velocities parallel to a background magnetic field. The whistler waves were launched and received by a pair of dipole antennas immersed in a cylindrical discharge plasma at two positions along an axial background magnetic field. The whistler wave frequency was swept from somewhat below and up to the electron cyclotron frequency {omega}{sub ce}. As the frequency was swept, the wave was resonantly absorbed by the part of the electron phase space density which was Doppler shifted into resonance according to the relation {omega}-k{sub ||v||} = {omega}{sub ce}. The measured absorption is directly related to the reduced parallel electron distribution function integrated along the wave trajectory. The background theory and initial results from this diagnostic are presented here. Though this diagnostic is best suited to detect tail populations of the parallel electron distribution function, these first results show that this diagnostic is also rather successful in measuring the bulk plasma density and temperature both during the plasma discharge and into the afterglow.

  8. Estimation of background gas concentration from differential absorption lidar measurements

    NASA Astrophysics Data System (ADS)

    Harris, Peter; Smith, Nadia; Livina, Valerie; Gardiner, Tom; Robinson, Rod; Innocenti, Fabrizio

    2016-10-01

    Approaches are considered to estimate the background concentration level of a target species in the atmosphere from an analysis of the measured data provided by the National Physical Laboratory's differential absorption lidar (DIAL) system. The estimation of the background concentration level is necessary for an accurate quantification of the concentration level of the target species within a plume, which is the quantity of interest. The focus of the paper is on methodologies for estimating the background concentration level and, in particular, contrasting the assumptions about the functional and statistical models that underpin those methodologies. An approach is described to characterise the noise in the recorded signals, which is necessary for a reliable estimate of the background concentration level. Results for measured data provided by a field measurement are presented, and ideas for future work are discussed.

  9. Determination of gold in geologic materials by solvent extraction and atomic-absorption spectrometry

    USGS Publications Warehouse

    Huffman, Claude; Mensik, J.D.; Riley, L.B.

    1967-01-01

    The two methods presented for the determination of traces of gold in geologic materials are the cyanide atomic-absorption method and the fire-assay atomic-absorption method. In the cyanide method gold is leached with a sodium-cyanide solution. The monovalent gold is then oxidized to the trivalent state and concentrated by extracting into methyl isobutyl ketone prior to estimation by atomic absorption. In the fire-assay atomic-absorption method, the gold-silver bead obtained from fire assay is dissolved in nitric and hydrochloric acids. Gold is then concentrated by extracting into methyl isobutyl ketone prior to determination by atomic absorption. By either method concentrations as low as 50 parts per billion of gold can be determined in a 15-gram sample.

  10. Thermodynamic Activity Measurements with Knudsen Cell Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Copland, Evan H.; Jacobson, Nathan S.

    2001-01-01

    Coupling the Knudsen effusion method with mass spectrometry has proven to be one of the most useful experimental techniques for studying the equilibrium between condensed phases and complex vapors. The Knudsen effusion method involves placing a condensed sample in a Knudsen cell, a small "enclosure", that is uniformly heated and held until equilibrium is attained between the condensed and vapor phases. The vapor is continuously sampled by effusion through a small orifice in the cell. A molecular beam is formed from the effusing vapor and directed into a mass spectrometer for identification and pressure measurement of the species in the vapor phase. Knudsen cell mass spectrometry (KCMS) has been used for nearly fifty years now and continues to be a leading technique for obtaining thermodynamic data. Indeed, much of the well-established vapor specie data in the JANAF tables has been obtained from this technique. This is due to the extreme versatility of the technique. All classes of materials can be studied and all constituents of the vapor phase can be measured over a wide range of pressures (approximately 10(exp -4) to 10(exp -11) bar) and temperatures (500-2800 K). The ability to selectively measure different vapor species makes KCMS a very powerful tool for the measurement of component activities in metallic and ceramic solutions. Today several groups are applying KCMS to measure thermodynamic functions in multicomponent metallic and ceramic systems. Thermodynamic functions, especially component activities, are extremely important in the development of CALPHAD (Calculation of Phase Diagrams) type thermodynamic descriptions. These descriptions, in turn, are useful for modeling materials processing and predicting reactions such as oxide formation and fiber/matrix interactions. The leading experimental methods for measuring activities are the Galvanic cell or electro-motive force (EMF) technique and the KCMS technique. Each has specific advantages, depending on

  11. Measurement of solutes in dialysate using UV absorption

    NASA Astrophysics Data System (ADS)

    Fridolin, Ivo; Magnusson, Martin; Lindberg, Lars-Goeran

    2001-06-01

    The aim of this work was to describe a new method for optical monitoring of solutes in a spent dialysate. The method utilizes UV light absorption employing a commercially available spectrophotometer. Measurements were performed both on collected dialysate samples and on-line. The concentration of several removed solutes and electrolytes in the serum and in the dialysate was determined simultaneously using standard laboratory techniques. During on-line monitoring the spectrophotometer was connected to the fluid outlet of the dialysis machine. On-line measurements during a single hemodialysis session demonstrated a possibility to monitor deviations in the dialysator performance (e.g. dialysator in by-pass). The experimental results indicated a good correlation between UV absorption and several removed solutes (urea, creatinine) in the spent dialysate. The correlation coefficient for urea and creatinine concentrations in the dialysate was very high for every individual treatment. The UV absorbance correlates well to the concentrations of several solutes thought to be uremic toxins. The results indicate that the technique can be used as a continuous, on-line method for monitoring deviations in the dialysator performance and may estimate the removal of the overall toxins. In the future, the new method will be used to evaluate parameters describing delivery of the prescribed treatment dose such as KT/V and Urea Reduction Rate (URR).

  12. Measurements of the absorption coefficient of stratospheric aerosols

    NASA Technical Reports Server (NTRS)

    Ogren, J. A.; Ahlquist, N. C.; Clarke, A. D.; Charlson, R. J.

    1981-01-01

    The absorption coefficients of stratospheric aerosols are measured using a variation on the integrating plate method. The technique is based on the decrease in the transparency of a substrate when an absorbing aerosol is deposited on it. A Lambert scatterer is placed behind the substrate to integrate forward scattered light and minimize the effect of scattering on the measurement. The low pressure in the stratosphere is used for the direct impaction of particles onto a narrow strip of opal glass. The eight samples collected had a median value of 4 x 10 to the -9th m with an uncertainty of + or - 5 x 10 to the -9th m. If this absorption is due to graphitic carbon, then its concentration is estimated at about 0.4 ng/cu m, or about 0.25% of the total aerosol mass concentration. Estimates of the aerosol scattering coefficients based on satellite extinction inversions result in an aerosol single-scattering albedo in the range of 0.96-1.0.

  13. Slurry sampling graphite furnace atomic absorption spectrometry: determination of trace metals in mineral coal.

    PubMed

    Silva, M M; Goreti, M; Vale, R; Caramão, E B

    1999-12-06

    A procedure for lead, cadmium and copper determination in coal samples based on slurry sampling using an atomic absorption spectrometer equipped with a transversely heated graphite tube atomizer is proposed. The slurries were prepared by weighing the samples directly into autosampler cups (5-30 mg) and adding a 1.5 ml aliquot of a diluent mixture of 5% v/v HNO(3), 0.05% Triton X-100 and 10% ethanol. The slurry was homogenized by manual stirring before measurement. Slurry homogenization using ultrasonic agitation was also investigated for comparison. The effect of particle size and the use of different diluent compositions on the slurry preparation were investigated. The temperature programmes were optimized on the basis of pyrolysis and atomization curves. Absorbance characteristics with and without the addition of a palladium-magnesium modifier were compared. The use of 0.05% m/v Pd and 0.03% m/v Mg was found satisfactory for stabilizing Cd and Pb. The calibration was performed with aqueous standards. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling. Better recoveries of the analytes were obtained when the particle size was reduced to <37 mum. Several certified coal reference materials (BCR Nos. 40, 180, and 181) were analyzed, and good agreement was obtained between the results from the proposed slurry sampling method and the certificate values.

  14. Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

    USGS Publications Warehouse

    Elsheimer, H.N.; Fries, T.L.

    1990-01-01

    A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

  15. Strontium mono-chloride - A new molecule for the determination of chlorine using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    NASA Astrophysics Data System (ADS)

    Pereira, Éderson R.; Welz, Bernhard; Lopez, Alfredo H. D.; de Gois, Jefferson S.; Caramori, Giovanni F.; Borges, Daniel L. G.; Carasek, Eduardo; de Andrade, Jailson B.

    2014-12-01

    A new method has been developed for the determination of chlorine in biological reference materials using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) of the strontium mono-chloride (SrCl) molecule and direct solid sample analysis. The use of the SrCl molecule for high-temperature MAS was not described up to now in the literature. Preliminary time-dependent density functional theory calculations of the SrCl structure were carried out in order to obtain reasonable estimates of the absorption spectrum of the target molecule. The calculations, which were carried out at BHandHLyp/def2-QZVP level of theory, proved a very accurate and inexpensive way to get information about the spectrum of the SrCl molecule, which enabled us to perform the Cl determination with good sensitivity and specificity. The molecular absorption of the SrCl molecule has been measured using the wavelength at 635.862 nm, and zirconium and palladium have been evaluated as the chemical modifiers in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Accuracy and precision of the method have been evaluated using biological certified reference materials of both animal and plant origins, showing good agreement with the informed and certified values. Limit of detection and characteristic mass were 1.0 and 2.2 ng, respectively. The results found using HR-CS GF MAS were in agreement (95% confidence level) compared to those obtained by electrothermal vaporization-inductively coupled plasma mass spectrometry.

  16. Measurement of Zinc Absorption From Meals: Comparison of Extrinsi Zinc Labeling and Independent Measurements of Dietary Zinc Absorption

    PubMed Central

    Sheng, Xiao-Yang; Hambidge, K. Michael; Miller, Leland V.; Westcott, Jamie E.; Lei, Sian; Krebs, Nancy F.

    2017-01-01

    Background Extrinsic labeling techniques are typically used to measure fractional absorption of zinc (FAZextrinsic) but none have been adequately evaluated. Objective To compare determination of the quantity of zinc absorbed (TAZextrinsic) using measurements of FAZextrinsic with results of simultaneous determinations of dietary zinc absorbed (TAZmetabolic) that are not dependent on labeling ingested food with an extrinsic tracer (modified metabolic balance technique). Design 70Zn was administered orally with all meals for 6 consecutive days to 21 healthy, free-living adult women consuming a constant diet. 68Zn and 67Zn were administered intravenously. FAZextrinsic was measured using a dual isotope tracer ratio technique and multiplied by dietary zinc to give TAZextrinsic TAZmetabolic was determined by addition of net absorption of zinc and endogenous fecal zinc, the latter determined by an isotope dilution technique. Results TAZextrinsic and TAZmetabolic were 3.0 ± 1.1mg/day and 3.1 ± 1.1 mg/day respectively, paired t-test p = 0.492. The correlation coefficient for TAZextrinsic and TAZmetabolic was 0.91, and for FAZextrinsic and FAZmetabolic was 0.95. A Bland Altman analysis indicated a bias of 0.07, and the limits of agreement of −0.86 to 1.01 for TAZextrinsic and TAZmatabolic Conclusion These results from two independent methods provide reasonable validation of our extrinsic labeling technique for a wide range of composite diets. PMID:20209474

  17. Determination of cadmium and lead in urine by derivative flame atomic absorption spectrometry using the atom trapping technique

    NASA Astrophysics Data System (ADS)

    Han-wen, Sun; De-qiang, Zhang; Li-li, Yang; Jian-min, Sun

    1997-06-01

    A method is described for the determinations of cadmium and lead in urine by derivative flame atomic absorption spectrometry with a modified water-cooled stainless steel atom trapping tube. The effects of the trap position, the flame conditions, the coolant flow rates, and the collection time were studied. With a 1 min collection time, the characteristic concentrations (derivative absorbance of 0.0044) for cadmium and lead were 0.028 and 1.4 μg L -1, the detection limits (3σ) were 0.02 and 0.27 μg L -1, respectively. The detection limits and sensitivities of the proposed method were 2 and 3 orders of magnitude higher for 1-3 min collection time than those of conventional flame atomic absorption spectrometry for cadmium and lead, respectively. Urine samples from a small population of normal individuals have been analyzed for cadmium and lead by the proposed method. Satisfactory recoveries of 91-110% and 91-106%, for Cd and Pb were obtained with these urine samples.

  18. Contents of cadmium, mercury and lead in fish from the Atlantic sea (Morocco) determined by atomic absorption spectrometry.

    PubMed

    Chahid, Adil; Hilali, Mustapha; Benlhachimi, Abdeljalil; Bouzid, Taoufiq

    2014-03-15

    As a part of a specific monitoring program, lead (Pb) cadmium (Cd) and mercury (Hg) concentrations in important species of fish from various fishing ports of the southern Kingdom of Morocco (Sardina pilchardus, Scomber scombrus, Plectorhinchus mediterraneus, Trachurus trachurus, Octopus vulgaris, Boops boops, Sarda sarda, Trisopterus capelanus, and Conger conger) were investigated by the Moroccan Reference Laboratory (NRL) for trace elements in foodstuffs of animal origin. The samples were analysed for lead and cadmium by a graphite furnace atomic absorption spectrometry (GFAAS); and for mercury by cold vapour atomic absorption spectrometry (CVAAS). The results were expressed as μg/g of wet weight (w/w). The levels of Cd, Pb and Hg in muscles of fish were 0.009-0.036, 0.013-0.114 and 0.049-0.194 μg/g, respectively. The present study showed that different metals were present in the sample at different levels but within the maximum residual levels prescribed by the EU for the fish and shellfish from these areas, in general, should cause no health problems for consumers.

  19. Determination of some trace elements in food and soil samples by atomic absorption spectrometry after coprecipitation with holmium hydroxide.

    PubMed

    Saracoglu, Sibel; Soylak, Mustafa; Cabuk, Dilek; Topalak, Zeynep; Karagozlu, Yasemin

    2012-01-01

    The determination of trace elements in food and soil samples by atomic absorption spectrometry was investigated. A coprecipitation procedure with holmium hydroxide was used for separation-preconcentration of trace elements. Trace amounts of copper(II), manganese(II), cobalt(II), nickel(ll), chromium(lll), iron(Ill), cadmium(ll), and lead(ll) ions were coprecipitated with holmium hydroxide in 2.0 M NaOH medium. The optimum conditions for the coprecipitation process were investigated for several commonly tested experimental parameters, such as amount of coprecipitant, effect of standing time, centrifugation rate and time, and sample volume. The precision, based on replicate analysis, was lower than 10% for the analytes. In order to verify the accuracy of the method, the certified reference materials BCR 141 R calcareous loam soil and CRM 025-050 soil were analyzed. The procedure was successfully applied for separation and preconcentration of the investigated ions in various food and soil samples. An amount of the solid samples was decomposed with 15 mL concentrated hydrochloric acid-concentrated nitric acid (3 + 1). The preconcentration procedure was then applied to the final solutions. The concentration of trace elements in samples was determined by atomic absorption spectrometry.

  20. Measurement of iron absorption from meals contaminated with iron

    SciTech Connect

    Hallberg, L.; Bjoern-Rasmussen, E.

    1981-12-01

    A method is described to measure in vitro the extent of isotopic exchange between the native nonheme food iron and added inorganic reduction to radioiron tracer. The food is digested with pepsin and trypsin in the presence of radioiron. The exchangeability of food iron is calculated from the specific activity in the food and in an extract of bathophenantroline in isoamyl alcohol obtained after digesting this food. The precision and accuracy of the method is illustrated by two kinds of studies, those in which different amounts of contamination iron are added to a meal and those evaluating contamination iron in natural meals. The present method will make it possible to measure validly iron absorption from meals contaminated with unknown amounts of iron of unknown exchangeability with the extrinsic radioiron tracer.

  1. Ultra sound absorption measurements in rock samples at low temperatures

    NASA Technical Reports Server (NTRS)

    Herminghaus, C.; Berckhemer, H.

    1974-01-01

    A new technique, comparable with the reverberation method in room acoustics, is described. It allows Q-measurements at rock samples of arbitrary shape in the frequency range of 50 to 600 kHz in vacuum (.1 mtorr) and at low temperatures (+20 to -180 C). The method was developed in particular to investigate rock samples under lunar conditions. Ultrasound absorption has been measured at volcanics, breccia, gabbros, feldspar and quartz of different grain size and texture yielding the following results: evacuation raises Q mainly through lowering the humidity in the rock. In a dry compact rock, the effect of evacuation is small. With decreasing temperature, Q generally increases. Between +20 and -30 C, Q does not change much. With further decrease of temperature in many cases distinct anomalies appear, where Q becomes frequency dependent.

  2. Ultraviolet absorption: Experiment MA-059. [measurement of atmospheric species concentrations

    NASA Technical Reports Server (NTRS)

    Donahue, T. M.; Hudson, R. D.; Rawlins, W. T.; Anderson, J.; Kaufman, F.; Mcelroy, M. B.

    1977-01-01

    A technique devised to permit the measurement of atmospheric species concentrations is described. This technique involves the application of atomic absorption spectroscopy and the quantitative observation of resonance fluorescence in which atomic or molecular species scatter resonance radiation from a light source into a detector. A beam of atomic oxygen and atomic nitrogen resonance radiation, strong unabsorbable oxygen and nitrogen radiation, and visual radiation was sent from Apollo to Soyuz. The density of atomic oxygen and atomic nitrogen between the two spacecraft was measured by observing the amount of resonance radiation absorbed when the line joining Apollo and Soyuz was perpendicular to their velocity with respect to the ambient atmosphere. Results of postflight analysis of the resonance fluorescence data are discussed.

  3. Phase measurement of fast light pulse in electromagnetically induced absorption.

    PubMed

    Lee, Yoon-Seok; Lee, Hee Jung; Moon, Han Seb

    2013-09-23

    We report the phase measurement of a fast light pulse in electromagnetically induced absorption (EIA) of the 5S₁/₂ (F = 2)-5P₃/₂ (F' = 3) transition of ⁸⁷Rb atoms. Using a beat-note interferometer method, a stable measurement without phase dithering of the phase of the probe pulse before and after it has passed through the EIA medium was achieved. Comparing the phases of the light pulse in air and that of the fast light pulse though the EIA medium, the phase of the fast light pulse at EIA resonance was not shifted and maintained to be the same as that of the free-space light pulse. The classical fidelity of the fast light pulse according to the advancement of the group velocity by adjusting the atomic density was estimated to be more than 97%.

  4. Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-07-20

    Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1).

  5. Separation and preconcentration of chromium species by selective absorption on Lemna minor and determination by slurry atomisation electrothermal atomic absorption spectrometry.

    PubMed

    Zhu, G; Li, S

    2001-08-01

    A novel method for the separation and preconcentration of Cr(III)/Cr(VI) with Lemna minor and determination by slurry atomization electrothermal atomic absorption spectrometry (ETAAS) was developed. A sample solution was added to a polyethylene beaker containing 10 mg of 160 mesh pre-treated Lemna minor, adjusted to pH 1.0, stirred for 8 min for selective absorption of Cr(III) and then centrifuged. The upper layer of solution was transferred into another polyethylene beaker containing 10 mg of 160 mesh pre-treated Lemna minor, adjusted to pH 5.0, stirred for 12 min for adsorption of the residual Cr(VI) and centrifuged. The two residues in two centrifuge tubes were washed twice with water, 2 ml of agar solution added, stirred for 2 min, then two slurries were prepared and used for the determination of Cr(III) and Cr(VI) by ETAAS. Detection limits (3sigma) of 0.01 microg L(-1) for Cr(III) and 0.03 microg L(-1) for Cr(VI) were obtained. The relative standard deviation was 2.8% for Cr(III) and 3.3% for Cr(VI) at the 1 microg L(-1) level. The method was applied to the determination of Cr(III)/Cr(VI) in water samples. The analytical recoveries of Cr(III) and Cr(VI) added to samples were 97-102 and 96-103%, respectively.

  6. Correlation between the Gas Temperature and the Atomization Behavior of Analyte Elements in Flame Atomic Absorption Spectrometry Estimated with a Continuum-light-source Spectrometer System

    NASA Astrophysics Data System (ADS)

    Toya, Yusuke; Itagaki, Toshiko; Wagatsuma, Kazuaki

    2016-11-01

    In flame atomic absorption spectrometry (FAAS), the gas temperature for two types of the gas compositions, which was estimated based on a two-line method by using a simultaneous multi-wavelength spectrometer, on which a line pair of ruthenium, Ru I 372.692 nm and Ru I 372.803 nm having different excitation energies, was measured at the same time. Also using the spectrometer system, the absorption signals of both iron and ruthenium, whose oxides had different thermodynamic properties: the latter oxide was decomposed much more easily than the former one, were investigated with a nitrous oxide - acetylene flame, in comparison with an air - acetylene flame. The fuel/oxidant ratio of both the flames as well as the height of the optical path was varied as an experimental parameter. The atomization behavior of iron and ruthenium, which could be deduced from a variation in their absorption signals, was considered to be dependent not only on the gas temperature but on reducing atmosphere of the flame gas, which might be attributed to reducing radicals in a fuel-excess flame consisting of nitrous oxide. In the nitrous oxide - acetylene flame, a broader optical path having a constant and higher temperature was obtained, thus contributing to formation of analyte atoms with a stable atomization efficiency and eventually to better precision in the analytical result in FAAS.

  7. Electrothermal atomization atomic absorption spectrometry for the determination of lead in urine: results of an interlaboratory study

    NASA Astrophysics Data System (ADS)

    Parsons, Patrick J.; Slavin, Walter

    1999-05-01

    Results of an interlaboratory study are reported for the determination of lead in urine. Two levels of a lyophilized material containing biologically-bound lead were prepared using pooled urine obtained from lead-poisoned children undergoing the CaNa 2EDTA mobilization test. The materials were circulated to a group of reference laboratories that participate in the `New York State Proficiency Testing Program for Blood Lead'. Results of the initial round-robin gave all-method consensus target values of 145±22 μg/l (S.D.) for lot 17 and 449±43 μg/l (S.D.) for lot 20. The interlaboratory exercise was repeated some 5 years later and consensus target values were re-calculated using the grand mean (excluding outliers) of results reported by laboratories using electrothermal atomization atomic absorption spectrometry (ETAAS). The re-calculated target values were 139±10 μg/l (S.D.) and 433±12 μg/l (S.D.). The urine reference materials were also analyzed for lead by several laboratories using other instrumental techniques including isotope dilution (ID), inductively coupled plasma (ICP) mass spectrometry (MS), flame atomic absorption with extraction, ICP-atomic emission spectrometry, ID-gas chromatography MS and flow injection-hydride generation AAS, thus providing a rich source of analytical data with which to characterize them. The materials were also used in a long-term validation study of an ETAAS method developed originally for blood lead determinations that has since been used unmodified for the determination of lead in urine also. Recently, urine lead method performance has been tracked in a proficiency testing program specifically for this analysis. In addition, a number of commercial control materials have been analyzed and evaluated.

  8. Chromium determination in pharmaceutical grade barium sulfate by solid sampling electrothermal atomic absorption spectrometry with Zeeman-effect background correction.

    PubMed

    Bolzan, Rodrigo Cordeiro; Rodrigues, Luis Frederico; Mattos, Júlio Cezar Paz de; Dressler, Valderi Luiz; Flores, Erico Marlon de Moraes

    2007-11-15

    A procedure for chromium (Cr) determination in pharmaceutical grade barium sulfate by direct solid sampling electrothermal atomic absorption spectrometry (DSS-ET AAS) with Zeeman-effect background correction was developed. Operational conditions for the proposed procedure and the use of citric acid, ammonium phosphate, palladium and magnesium nitrate as chemical modifiers were evaluated. Pyrolysis and atomization temperatures were set at 1500 and 2400 degrees C, respectively and the use of matrix modifiers did not improve these conditions. Graphite platform presented high degradation rate, but minima changes were observed in the sensitivity or signal profile. Samples (0.3-1 mg) were weighted and introduced into the furnace using a manual solid sampling system. The linear concentration range of the calibration curve was from 100 to 1800 pg (R(2)>0.995). The characteristic mass was 7.7 pg and the limit of detection was 2.4 pg. Chromium concentration in commercial samples ranged from 0.45 to 1.06 microg g(-1) and these results were confirmed by standard addition method. The mean reproducibility was 12% (n=20 in a 3-day period) and repeatability was less than 9%. Results obtained using inductively coupled plasma optical emission spectrometry and conventional electrothermal atomic absorption spectrometry after extraction with HNO3 were around 20% lower than those obtained by the proposed procedure. It was assumed that the low results were due to incomplete extraction even using hard conditions related to temperature and pressure. The proposed procedure by DSS-ET AAS provided some advantages related to recommended pharmacopoeias methodology, as lower risks of contamination and analyte losses, higher specificity, accuracy and sensitivity, no toxic or unstable reagents are required, and calibration with aqueous standards was feasible.

  9. Ambient Ionization Mass Spectrometry Measurement of Aminotransferase Activity

    NASA Astrophysics Data System (ADS)

    Yan, Xin; Li, Xin; Zhang, Chengsen; Xu, Yang; Cooks, R. Graham

    2017-01-01

    A change in enzyme activity has been used as a clinical biomarker for diagnosis and is useful in evaluating patient prognosis. Current laboratory measurements of enzyme activity involve multi-step derivatization of the reaction products followed by quantitative analysis of these derivatives. This study simplified the reaction systems by using only the target enzymatic reaction and directly detecting its product. A protocol using paper spray mass spectrometry for identifying and quantifying the reaction product has been developed. Evaluation of the activity of aspartate aminotransferase (AST) was chosen as a proof-of-principle. The volume of sample needed is greatly reduced compared with the traditional method. Paper spray has a desalting effect that avoids sprayer clogging problems seen when examining serum samples by nanoESI. This very simple method does not require sample pretreatment and additional derivatization reactions, yet it gives high quality kinetic data, excellent limits of detection (60 ppb from serum), and coefficients of variation <10% in quantitation.

  10. Spectral Measurements of Aerosol Absorption from UV to VISIBLE

    NASA Astrophysics Data System (ADS)

    Krotkov, N. A.; Labow, G.; Herman, J.; Bhartia, P. K.; Slusser, J.; Durham, B.; Janson, G.; Wilson, C.; Disterhoft, P.; Cede, A.; Abuhassan, N.; Eck, T. F.; Holben, B.; Bais, A.; Rapsomanikis, S.

    2007-05-01

    Amount of solar radiation reaching the Earth's surface can be strongly influenced by aerosol absorption. The aerosol absorption optical thickness (AAOT) in the visible and near IR (440 nm- 1020nm) is routinely produced from almucantar measurements made by the CIMEL instruments in the AERONET network. AAOT in the UV (300nm- 368nm) have been derived from the total and diffuse hemispherical flux measurements made by UV- Multifilter Rotating Shadowband Radiometer (UV-MFRSR, Yankee Environmental Systems, Inc.) instruments. However, no direct comparisons between these two methods exist because the CIMEL wavelengths (used in almucantar retrievals) do not overlap with the UV-MFRSR wavelengths. To enable direct comparisons between the two techniques, we have modified our UV-MFRSR, part of USDA UVB Monitoring and Research Network, by replacing standard 300nm filter with 440nm filter used in AERONET network. The instrument has been deployed at Mauna Loa Observatory, at NASA GSFC in Greenbelt, MD (July 2005 - June 2006) and during SCOUT-03 field campaign in Thessaloniki, Greece in July 2006. During these deployments the instrument's calibration was monitored daily using co-located AERONET and BREWER direct sun measurements of aerosol extinction optical thickness (AOT). Between the deployments the instrument was thoroughly calibrated at the NOAA Central UV Calibration Facility in Boulder, Colorado. We find that the UV-MSFRSR instrument is highly susceptible to calibration drifts. However, these drifts can be accurately assessed using AERONET and BREWER direct sun data. After correcting for these calibration changes, the AAOT was inferred by fitting the measurements of global and diffuse atmospheric transmittances with the forward RT model independently at each spectral channel. The AOT data and ancillary measurements of aerosol column particle size distribution and refractive index in the visible wavelengths (by CIMEL sun-sky almucantar inversions), direct -sun column NO2 and

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

  12. Slurry sampling for direct analysis of solid materials by electrothermal atomic absorption spectrometry (ETAAS). A literature review from 1990 to 2000.

    PubMed

    Cal-Prieto, M J; Felipe-Sotelo, M; Carlosena, A; Andrade, J M; López-Mahía, P; Muniategui, S; Prada, D

    2002-01-04

    The determination of trace metals in solid samples has traditionally been performed by acid digestion and subsequent measurement by a suitable instrumental technique. This dissolution step is time-consuming and it shows important drawbacks. For these reasons, in the past years many efforts have been focused on the direct analysis of solid samples. Among the developed methodologies, slurry sampling-electrothermal atomic absorption spectrometry combines the significant advantages of the solid and liquid sampling methods, and it can be already considered as a mature technique, that is widely utilized for metal determination in both organic and inorganic matrices, even for routine analysis. Accordingly, this work gives a retrospective view of the progresses of this technique during the past decade (1990-2000).

  13. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    NASA Astrophysics Data System (ADS)

    Kruger, Pamela C.; Parsons, Patrick J.

    2007-03-01

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass ( m0), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 ± 0.6 pg, compared to 16.1 ± 0.7 pg for the Z5100, and 23.3 ± 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection limits (3

  14. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

  15. Radionuclide measurements by accelerator mass spectrometry at Arizona

    NASA Technical Reports Server (NTRS)

    Jull, A. J. T.; Donahue, D. J.; Zabel, T. H.

    1986-01-01

    Over the past years, Tandem Accelerator Mass Spectrometry (TAMS) has become established as an important method for radionuclide analysis. In the Arizona system the accelerator is operated at a thermal voltage of 1.8MV for C-14 analysis, and 1.6 to 2MV for Be-10. Samples are inserted into a cesium sputter ion source in solid form. Negative ions sputtered from the target are accelerated to about 25kV, and the injection magnet selects ions of a particular mass. Ions of the 3+ charge state, having an energy of about 9MeV are selected by an electrostatic deflector, surviving ions pass through two magnets, where only ions of the desired mass-energy product are selected. The final detector is a combination ionization chamber to measure energy loss (and hence, Z), and a silicon surface-barrier detector which measures residual energy. After counting the trace iosotope for a fixed time, the injected ions are switched to the major isotope used for normalization. These ions are deflected into a Faraday cup after the first high-energy magnet. Repeated measurements of the isotope ratio of both sample and standards results in a measurement of the concentration of the radionuclide. Recent improvements in sample preparation for C-14 make preparation of high-beam current graphite targets directly from CO2 feasible. Except for some measurements of standards and backgrounds for Be-10 measurements to date have been on C-14. Although most results have been in archaeology and quaternary geology, studies have been expanded to include cosmogenic C-14 in meteorites. The data obtained so far tend to confirm the antiquity of Antarctic meteorites from the Allan Hills site. Data on three samples of Yamato meteorites gave terrestrial ages of between about 3 and 22 thousand years.

  16. Contact sponge water absorption test implemented for in situ measures

    NASA Astrophysics Data System (ADS)

    Gaggero, Laura; Scrivano, Simona

    2016-04-01

    The contact sponge method is a non-destructive in-situ methodology used to estimate a water uptake coefficient. The procedure, unlike other in-situ measurement was proven to be directly comparable to the water uptake laboratory measurements, and was registered as UNI 11432:2011. The UNI Normal procedure requires to use a sponge with known density, soaked in water, weighed, placed on the material for 1 minute (UNI 11432, 2011; Pardini & Tiano, 2004), then weighed again. Difficulties arise in operating on test samples or on materials with porosity varied for decay. While carrying on the test, fluctuations in the bearing of the environmental parameters were negligible, but not the pressure applied to the surface, that induced the release of different water amounts towards the material. For this reason we designed a metal piece of the same diameter of the plate carrying the sponge, to be screwed at the tip of a pocket penetrometer. With this instrument the sponge was kept in contact with the surface for 1 minute applying two different loads, at first pushed with 0.3 kg/cm2 in order to press the sponge, but not its holder, against the surface. Then, a load of 1.1 kg/ cm2 was applied, still avoiding deviating the load to the sponge holder. We applied both the current and our implemented method to determine the water absorption by contact sponge on 5 fresh rock types (4 limestones: Fine - and Coarse grained Pietra di Vicenza, Rosso Verona, Breccia Aurora, and the silicoclastic Macigno sandstone). The results show that 1) the current methodology imply manual skill and experience to produce a coherent set of data; the variable involved are in fact not only the imposed pressure but also the compression mechanics. 2) The control on the applied pressure allowed reproducible measurements. Moreover, 3) the use of a thicker sponge enabled to apply the method even on rougher surfaces, as the device holding the sponge is not in contact with the tested object. Finally, 4) the

  17. High resolution Fourier transform spectrometry in emission and absorption in the visible and UV ranges

    NASA Astrophysics Data System (ADS)

    Luc, Paul

    1995-07-01

    This paper gives the main results obtained at Laboratoire Aimé Cotton, using Fourier transform spectroscopy (FTS) in the visible and UV ranges. After a rapid historical survey, a description of the fourth generation interferometer, which is specially designed to record visible and UV light will be given. Typical results in emission and absorption spectroscopy, including the metrological applications, will follow.

  18. Extraction of full absorption peaks in airborne gamma-spectrometry by filtering techniques coupled with a study of the derivatives. Comparison with the window method.

    PubMed

    Guillot, L

    2001-01-01

    In this paper, an adaptation of a spectral profile analysis method, currently used in high-resolution spectrometry, to airborne gamma measurements is presented. A new algorithm has been developed for extraction of full absorption peaks by studying the variations in the spectral profile of data recorded with large-volume NaI detectors (16 l) with a short sampling time (2 s). The use of digital filters, taking into consideration the characteristics of the absorption peaks, significantly reduced the counting fluctuations, making detection possible based on study of the first and second derivatives. The absorption peaks are then obtained by modelling, followed by subtraction of the Compton continuum in the detection window. Compared to the conventional stripping ratio method, spectral profile analysis offers similar performance for the natural radioelements. The 137Cs 1SD detection limit is approximately 1200 Bq/m2 in a natural background of 200 Bq/kg 40K, 33 Bq/kg 238U and 33 Bq/kg 232Th. At low energy the very high continuum leads to detection limits similar to those obtained by the windows method, but the results obtained are more reliable. In the presence of peak overlaps, however, analysis of the spectral profile alone is not sufficient to separate the peaks, and further processing is necessary. Within the framework of environmental monitoring studies, spectral profile analysis is of great interest because it does not require any assumptions about the nature of the nuclides. The calculation of the concentrations from the results obtained is simple and reliable, since only the full absorption contributions are taken into consideration. A quantitative estimate of radioactive anomalies can thus be obtained rapidly.

  19. Method for improving terahertz band absorption spectrum measurement accuracy using noncontact sample thickness measurement.

    PubMed

    Li, Zhi; Zhang, Zhaohui; Zhao, Xiaoyan; Su, Haixia; Yan, Fang; Zhang, Han

    2012-07-10

    The terahertz absorption spectrum has a complex nonlinear relationship with sample thickness, which is normally measured mechanically with limited accuracy. As a result, the terahertz absorption spectrum is usually determined incorrectly. In this paper, an iterative algorithm is proposed to accurately determine sample thickness. This algorithm is independent of the initial value used and results in convergent calculations. Precision in sample thickness can be improved up to 0.1 μm. A more precise absorption spectrum can then be extracted. By comparing the proposed method with the traditional method based on mechanical thickness measurements, quantitative analysis experiments on a three-component amino acid mixture shows that the global error decreased from 0.0338 to 0.0301.

  20. Measuring Food Intake and Nutrient Absorption in Caenorhabditis elegans.

    PubMed

    Gomez-Amaro, Rafael L; Valentine, Elizabeth R; Carretero, Maria; LeBoeuf, Sarah E; Rangaraju, Sunitha; Broaddus, Caroline D; Solis, Gregory M; Williamson, James R; Petrascheck, Michael

    2015-06-01

    Caenorhabditis elegans has emerged as a powerful model to study the genetics of feeding, food-related behaviors, and metabolism. Despite the many advantages of C. elegans as a model organism, direct measurement of its bacterial food intake remains challenging. Here, we describe two complementary methods that measure the food intake of C. elegans. The first method is a microtiter plate-based bacterial clearing assay that measures food intake by quantifying the change in the optical density of bacteria over time. The second method, termed pulse feeding, measures the absorption of food by tracking de novo protein synthesis using a novel metabolic pulse-labeling strategy. Using the bacterial clearance assay, we compare the bacterial food intake of various C. elegans strains and show that long-lived eat mutants eat substantially more than previous estimates. To demonstrate the applicability of the pulse-feeding assay, we compare the assimilation of food for two C. elegans strains in response to serotonin. We show that serotonin-increased feeding leads to increased protein synthesis in a SER-7-dependent manner, including proteins known to promote aging. Protein content in the food has recently emerged as critical factor in determining how food composition affects aging and health. The pulse-feeding assay, by measuring de novo protein synthesis, represents an ideal method to unequivocally establish how the composition of food dictates protein synthesis. In combination, these two assays provide new and powerful tools for C. elegans research to investigate feeding and how food intake affects the proteome and thus the physiology and health of an organism.

  1. Laser induced deflection technique for absolute thin film absorption measurement: optimized concepts and experimental results

    SciTech Connect

    Muehlig, Christian; Kufert, Siegfried; Bublitz, Simon; Speck, Uwe

    2011-03-20

    Using experimental results and numerical simulations, two measuring concepts of the laser induced deflection (LID) technique are introduced and optimized for absolute thin film absorption measurements from deep ultraviolet to IR wavelengths. For transparent optical coatings, a particular probe beam deflection direction allows the absorption measurement with virtually no influence of the substrate absorption, yielding improved accuracy compared to the common techniques of separating bulk and coating absorption. For high-reflection coatings, where substrate absorption contributions are negligible, a different probe beam deflection is chosen to achieve a better signal-to-noise ratio. Various experimental results for the two different measurement concepts are presented.

  2. Quantitative measurement of endogenous amino acid absorption in unanaesthetized pigs.

    PubMed

    Rerat, A; Vaissade, P; Vaugelade, P

    1988-06-01

    The present experiment was carried out with 11 pigs (mean body weight: 53.9 +/- 1.3 kg) fitted with permanent catheters in the portal vein and carotid artery and with an electromagnetic flow probe around the portal vein. They were each subjected to 2 or 3 trials at 3 to 4-day intervals. During each trial the animals received after a previous fasting of 20 h a given amount of a protein-free diet (200 to 1200 g). The blood was collected either continuously for a quantitative determination of amino nitrogen, reducing sugars, urea and ammonia (number of meals 12, mean intake: 727 +/- 60 g) or discontinuously every 30 min between 0 and 8 h after the meal for amino acid analysis (number of meals 8; mean intake 709 +/- 105 g). A rather constant appearance (2 g/h) of amino acids in the portal blood was observed throughout the postprandial period. The intestinal absorption of each amino acid was however variable and represented between 10 and 50% of the daily requirements of the animal during the measuring period (8 h). Glutamine and to a less extent glutamic acid were exceptions as they were taken up by the gut wall from the arterial blood. There was also a marked synthesis of ornithine and citrulline by the latter. Because of the low blood level of urea, there were no apparent exchanges of urea between the blood and the intestine; in contrast, the ammonia absorption represented about 70% of that observed after ingestion of normal protein diets. Most amino acids are largely taken up by the liver and peripheral tissues, but in the case of alanine the syntheses exceed the uptake.

  3. The application of solid sorbents for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry.

    PubMed

    Bulska, E; Pyrzyńska, K

    1996-06-01

    Various microcolumns with solid sorbents (ion exchange resins, functionalised cellulose sorbents, chelating resins) have been tested with respect to their ability for the purification of aluminum contaminated chemicals used as modifiers in electrothermal atomic absorption spectrometry. The purification of NaNO(3), Mg(NO(3))(2), K(2)SO(4) and (NH(4))(2)HPO(4) has been the most effective with an almost 100% efficiency, when Spheron-Oxine was used as chelating resin. The sorption of aluminum from KOH solution has been found to be very high (around 90%) for all investigated sorbents. However, the best results have been obtained with anion-exchange resins. It has been difficult to purify concentrated mineral acids (HCl, H(2)SO(4)). A retention of aluminum above 80% has been achieved only when Cellex P, Chelex 100 or Amberlite XAD-2 have been used.

  4. Determination of total mercury in environmental and biological samples by flow injection cold vapour atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Murphy, James; Jones, Phil; Hill, Steve J.

    1996-12-01

    A simple and accurate method has been developed for the determination of total mercury in environmental and biological samples. The method utilises an off-line microwave digestion stage followed by analysis using a flow injection system with detection by cold vapour atomic absorption spectrometry. The method has been validated using two certified reference materials (DORM-1 dogfish and MESS-2 estuarine sediment) and the results agreed well with the certified values. A detection limit of 0.2 ng g -1 Hg was obtained and no significant interference was observed. The method was finally applied to the determination of mercury in river sediments and canned tuna fish, and gave results in the range 0.1-3.0 mg kg -1.

  5. Diagnostics of reactive pulsed plasmas by UV and VUV absorption spectroscopy and by modulated beam Mass spectrometry

    NASA Astrophysics Data System (ADS)

    Cunge, Gilles

    2011-10-01

    Pulsed plasmas are promising for etching applications in the microelectronic industry. However, many new phenomena are involved when a high density discharge is pulsed. To better understand these processes it is necessary to probe the radicals' kinetics with a microsecond resolution. We have developed several diagnostics to reach this goal including broad band absorption spectroscopy with UV LEDs to detect small polyatomic radicals and with a deuterium VUV source to detect larger closed shell molecules and the modulated mass spectrometry to monitor atomic species. We will discuss the impact of the plasma pulsing frequency and duty cycle on the radical densities in Cl2 based plasmas, and the consequences on plasma processes. Work done in collaboration with Paul Bodart, Melisa Brihoum, Maxime Darnon, Erwin Pargon, Olivier Joubert, and Nader Sadeghi, CNRS/LTM.

  6. Determination of arsenic, antimony, bismuth, cadmium, copper, lead, molybdenum, silver and zinc in geological materials by atomic-absorption spectrometry

    USGS Publications Warehouse

    Viets, J.G.; O'Leary, R. M.; Clark, Robert J.

    1984-01-01

    Arsenic, antimony, bismuth, cadmium, copper, lead, molybdenum, silver and zinc are very useful elements in geochemical exploration. In the proposed method, geological samples are fused with potassium pyrosulphate and the fusate is dissolved in a solution of hydrochloric acid, ascorbic acid and potassium iodide. When this solution is shaken with a 10% V/V Aliquat 336 - isobutyl methyl ketone organic phase, the nine elements of interest are selectively partitioned in the organic phase. All nine elements can then be determined in the organic phase using flame atomic-absorption spectrometry. The method is rapid and allows the determination of Ag and Cd at levels down to 0.1 p.p.m., Cu, Mo, and Zn down to 0.5 p.p.m., Pb, Bi and Sb down to 1 p.p.m. and As down to 5 p.p.m. in geological materials.

  7. Impact of the analytical blank in the uncertainty evaluation of the copper content in waters by flame atomic absorption spectrometry.

    PubMed

    de Oliveira, Elcio Cruz; Monteiro, Maria Inês Couto; Pontes, Fernanda Veronesi Marinho; de Almeida, Marcelo Dominguez; Carneiro, Manuel Castro; da Silva, Lílian Irene Dias; Alcover Neto, Arnaldo

    2012-01-01

    Chemical analysts use analytical blanks in their analyses, but seldom is this source of uncertainty evaluated. Generally, there is great confusion. Although the numerical value of the blank, in some situations, can be negligible, its source of uncertainty cannot be. This article discusses the uncertainty contribution of the analytical blank using a numerical example of the copper content in waters by flame atomic absorption spectrometry. The results indicate that the uncertainties of the analytical blank can contribute up to 50% when the blank sample is considered in this analysis, confirming its high impact. This effect can be primarily observed where the analyte concentration approaches the lower range of the analytical curve. Even so, the blank is not always computed. Therefore, the relevance of the analytical blank can be confirmed by uncertainty evaluation.

  8. Determination of bismuth in environmental samples by slurry sampling graphite furnace atomic absorption spectrometry using combined chemical modifiers.

    PubMed

    Dobrowolski, Ryszard; Dobrzyńska, Joanna; Gawrońska, Barbara

    2015-01-01

    Slurry sampling graphite furnace atomic absorption spectrometry technique was applied for the determination of Bi in environmental samples. The study focused on the effect of Zr, Ti, Nb and W carbides, as permanent modifiers, on the Bi signal. Because of its highest thermal and chemical stability and ability to substantially increase Bi signal, NbC was chosen as the most effective modifier. The temperature programme applied for Bi determination was optimized based on the pyrolysis and atomization curves obtained for slurries prepared from certified reference materials (CRMs) of the soil and sediments. To overcome interferences caused by sulfur compounds, Ba(NO₃)₂ was used as a chemical modifier. Calibration was performed using the aqueous standard solutions. The analysis of the CRMs confirmed the reliability of the proposed analytical method. The characteristic mass for Bi was determined to be 16 pg with the detection limit of 50 ng/g for the optimized procedure at the 5% (w/v) slurry concentration.

  9. Determination of silver, bismuth, cadmium, copper, lead, and zinc in geologic materials by atomic absorption spectrometry with tricaprylylmethylammonium chloride

    USGS Publications Warehouse

    Viets, J.G.

    1978-01-01

    Interferences commonly encountered in the determination of silver, bismuth, cadmium, copper, lead, and zinc at crustal abundance levels are effectively eliminated using a rapid, sensitive, organic extraction technique. A potassium chlorate-hydrochloric acid digestion solubilizes the metals not tightly bound in the silicate lattice of rocks, soils, and stream sediments. The six metals are selectively extracted into a 10% Aliquat 336-MIBK organic phase in the presence of ascorbic acid and potassium iodide. Metals in the organic extract are determined by flame atomic absorption spectrometry to the 0.02-ppm level for silver, cadmium, copper, and zinc and to the 0.2-ppm level for bismuth and lead with a maximum relative standard deviation of 18.8% for known reference samples. An additional hydrofluoric acid digestion may be used to determine metals substituted in the silicate lattice.

  10. Determination of chromium, manganese and vanadium in sediments and soils by modifier—free slurry sampling electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mierzwa, J.; Sun, Yuh-Chang; Yang, Mo-Hsiung

    1998-01-01

    Slurried sediment and soil samples of the certified reference materials with a highly elevated level of the metals of interest (Mn, Cr and V) were analysed by electrothermal atomic absorption spectrometry (ETAAS) with Zeeman effect background correction. The method of slurry preparation and time-temperature programmes were optimized and, finally, the use of chemical modifiers was not necessary. The effect of alternate spectral lines and gas mini-flows on characteristic masses of analytes was studied. The homogeneity of samples and the influence of short sample grinding were also discussed. The simple, aqueous standard based calibration graphs (except Mn at the concentration > 1000 mg kg -1) were applied for the quantification of results. The results of determinations obtained by slurry sampling agreed well with the cetified values, and the relative standard deviations (RSDs) for the over-all analytical procedure repeatability (at slurries concentration level about 2 mg/2 ml) were less than 9.5%, except manganese (10.4%).

  11. A new approach to mineralization of flaxseed (Linum usitatissimum L.) for trace element analysis by flame atomic absorption spectrometry.

    PubMed

    Oliveira, João P S; Silva, Francisco L F; Monte, Raimundo J G; Matos, Wladiana O; Lopes, Gisele S

    2017-06-01

    A new approach to the analysis of Cu, Fe, Mn and Zn in flaxseed was developed based on infrared-assisted acid digestion. Quantitation by flame atomic absorption spectrometry yields results in agreement with those arising from aggressive total decomposition using conventional microwave-assisted (MW) digestions. A full factorial design in two levels was applied to evaluate the impact of significant variables for all elements to determine optimal experimental conditions. A desirability function revealed these to be: 2.0g sample mass, 8mL of HNO3 and 8min of heating time in the IR system. Precision better than 10% (RSD) was obtained, superior to that of a combined IR-MW approach. Sample preparation based on IR-assisted digestion provides a rapid and inexpensive alternative to other conventional techniques for the analysis of complex samples and is able to accommodate relatively large masses of sample, alleviating potential homogeneity issues as well as enhancing detection power.

  12. Determination of cadmium by electrothermal atomic absorption spectrometry after microwave-assisted digestion of animal tissues and sewage sludges.

    PubMed

    Chakraborty, R; Das, A K; Cervera, M L; De La Guardia, M

    1996-04-01

    The determination of cadmium in different sample types has been carried out by electrothermal atomization atomic absorption spectrometry with D(2)-background correction using a unpyrocoated graphite tube, after pressurized microwave-assisted digestion. Five chemical modifiers [(NH(4))(2)HPO(4), Pd(NO)(3))(2), Ni(NO(3))(2), thiourea and Triton X-100] have been assayed and nickel nitrate has been found to be most effective for an accurate determination of cadmium in mussel tissue, pig kidney and sewage sludge. The characteristic mass of the method is of the order of 1 pg and the limit of detection is lower than 0.1 ng/ml.

  13. Determination of cadmium in spring water by graphite-furnace atomic absorption spectrometry after coprecipitation with ytterbium hydroxide.

    PubMed

    Atsumi, Kousuke; Minami, Tomoharu; Ueda, Joichi

    2005-06-01

    A coprecipitation method with ytterbium hydroxide was studied for the determination of cadmium in water samples by graphite-furnace atomic absorption spectrometry. Up to 40 ng of cadmium in water samples was quantitatively coprecipitated with ytterbium hydroxide at pH 8.0-11.2. The concentration factor was 100 fold. The coprecipitated cadmium was sensitively determined without any influence of ytterbium and the calibration curve was linear from 0.1 to 4 ng/mL of cadmium. The detection limit (signal/noise = 2) was 2.9 pg/mL in 100 mL of the initial sample solution. Twenty-nine diverse ions tested did not interfere with the determination in at least a 10000-fold mass ratio to cadmium. The proposed method was successfully applied to the determination of cadmium in spring water.

  14. FemtoMolar measurements using accelerator mass spectrometry.

    PubMed

    Salehpour, Mehran; Forsgard, Niklas; Possnert, Göran

    2009-03-01

    Accelerator mass spectrometry (AMS) is an ultra-sensitive analytical method suitable for the detection of sub-nM concentrations of labeled biological substances such as pharmaceutical drugs in body fluids. A limiting factor in extending the concentration measurements to the sub-pM range is the natural (14)C content in living tissues. This was circumvented by separating the labeled drug from the tissue matrix, using standard high-performance liquid chromatography (HPLC) procedures. As the separated total drug amount is in the few fg range, it is not possible to use a standard AMS sample preparation method, where mg sizes are required. We have utilized a sensitive carbon carrier method where a (14)C-deficient compound is added to the HPLC fractions and the composite sample is prepared and analyzed by AMS. Using 50 microL human blood plasma aliquots, we have demonstrated concentration measurements below 20 fM, containing sub-amol amounts of the labeled drug. The method has the immediate potential of operating in the sub-fM region.

  15. Nanowire dopant measurement using secondary ion mass spectrometry

    SciTech Connect

    Chia, A. C. E.; Boulanger, J. P.; Wood, B. A.; LaPierre, R. R.; Dhindsa, N.; Saini, S. S.

    2015-09-21

    A method is presented to improve the quantitative determination of dopant concentration in semiconductor nanowire (NW) arrays using secondary ion mass spectrometry (SIMS). SIMS measurements were used to determine Be dopant concentrations in a Be-doped GaAs thin film and NW arrays of various pitches that were dry-etched from the same film. A comparison of these measurements revealed a factor of 3 to 12 difference, depending on the NW array pitch, between the secondary Be ion yields of the film and the NW arrays, despite being identically doped. This was due to matrix effects and ion beam mixing of Be from the NWs into the surrounding benzocyclobutene that was used to fill the space between the NWs. This indicates the need for etched NWs to be used as doping standards instead of 2D films when evaluating NWs of unknown doping by SIMS. Using the etched NWs as doping standards, NW arrays of various pitches grown by the vapour-liquid-solid mechanism were characterized by SIMS to yield valuable insights into doping mechanisms.

  16. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    NASA Astrophysics Data System (ADS)

    Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; da Silva, Alessandra Furtado; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson José

    2005-06-01

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 °C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 °C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1.

  17. Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero

    2014-11-01

    The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption-elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L- 1, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64-22.9 μg Pb L- 1).

  18. A simple and fast method for assessment of the nitrogen-phosphorus-potassium rating of fertilizers using high-resolution continuum source atomic and molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Bechlin, Marcos André; Fortunato, Felipe Manfroi; da Silva, Ricardo Moutinho; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta

    2014-11-01

    The determination of N, P, and K in fertilizers by high-resolution continuum source flame atomic and molecular absorption spectrometry is proposed. Under optimized conditions, measurements of the diatomic molecules NO and PO at 215.360 and 247.620 nm, respectively, and K using the wing of the alternative line at 404.722 nm allowed calibration curves to be constructed in the ranges 500-5000 mg L- 1 N (r = 0.9994), 100-2000 mg L- 1 P (r = 0.9946), and 100-2500 mg L- 1 K (r = 0.9995). Commercial fertilizers were analyzed by the proposed method and the concentrations of N, P, and K were found to be in agreement with those obtained by Kjeldahl, spectrophotometric, and flame atomic emission spectrometry methods, respectively, at a 95% confidence level (paired t-test). A phosphate rock certified reference material (CRM) was analyzed and the results for P and K were in agreement with the reference values. Recoveries from spiked CRM were in the ranges 97-105% (NO3--N), 95-103% (NH4+-N), 93-103% (urea-N), 99-108% (P), and 99-102% (K). The relative standard deviations (n = 12) for N, P, and K were 6, 4, and 2%, respectively.

  19. Determination of boron in silicon-doped gallium arsenide by electrothermal atomic absorption spectrometry and ultraviolet-visible spectrophotometry.

    PubMed

    Taddia, Marco; Cerroni, Maria Grazia; Morelli, Elio; Musiani, Andrea

    2002-01-01

    Two methods have been developed for the determination of boron impurities in silicon-doped gallium arsenide (GaAs) for electronics. The first method employs the electrothermal atomic absorption spectrometry (ETAAS), the second, the UV-Vis molecular absorption spectrophotomety. In both cases the GaAs sample is decomposed with aqua regia (1+1). To prevent Ga(III) interference on the ETAAS determination of boron, a double extraction of the chlorogallic acid (HGaCl4) in diethyl ether is performed. To improve the overall ETAAS performance, the graphite tubes were pre-treated with iridium(III) and tungsten(IV). A mixed chemical modifier containing Ni(II), Sr(II) and citric acid was also used. The characteristic mass (m0) is 301 +/- 47 pg and the detection limit (3sB) is 2.4 microg g(-1). The classic UV-Vis spectrophotometric procedure using curcumin was also extended to the determination of boron in GaAs. By masking Ga(III) with EDTA and a preliminary extraction of boron with 2-ethyl-hexane 1,3-diol, performed on a semi-micro scale, a detection limit of 0.6 microg g(-1) was achieved. Both methods were applied to the analysis of two Si-doped GaAs samples which were suspected of being boron-contaminated. Results are compared with those obtained by direct analysis of the decomposed sample solution using the inductively coupled plasma atomic emission spectrometry (ICP-AES).

  20. Direct determination of Cu, Mn, Pb, and Zn in beer by thermospray flame furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Nascentes, Clésia C.; Kamogawa, Marcos Y.; Fernandes, Kelly G.; Arruda, Marco A. Z.; Nogueira, Ana Rita A.; Nóbrega, Joaquim A.

    2005-06-01

    In this work, thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was employed for Cu, Mn, Pb, and Zn determination in beer without any sample digestion. The system was optimized and calibration was based on the analyte addition technique. A sample volume of 300 μl was introduced into the hot Ni tube at a flow-rate of 0.4 ml min -1 using 0.14 mol l -1 nitric acid solution or air as carrier. Different Brazilian beers were directly analyzed after ultrasonic degasification. Results were compared with those obtained by graphite furnace atomic absorption spectrometry (GFAAS). The detection limits obtained for Cu, Mn, Pb, and Zn in aqueous solution were 2.2, 18, 1.6, and 0.9 μg l -1, respectively. The relative standard deviations varied from 2.7% to 7.3% ( n=8) for solutions containing the analytes in the 25-50 μg l -1 range. The concentration ranges obtained for analytes in beer samples were: Cu: 38.0-155 μg l -1; Mn: 110-348 μg l -1, Pb: 13.0-32.9 μg l -1, and Zn: 52.7-226 μg l -1. Results obtained by TS-FF-AAS and GFAAS were in agreement at a 95% confidence level. The proposed method is fast and simple, since sample digestion is not required and sensitivity can be improved without using expensive devices. The TS-FF-AAS presented suitable sensitivity for determination of Cu, Mn, Pb, and Zn in the quality control of a brewery.

  1. Fast sequential determination of antimony and lead in pewter alloys using high-resolution continuum source flame atomic absorption spectrometry.

    PubMed

    Dessuy, Morgana B; de Jesus, Robson M; Brandao, Geovani C; Ferreira, Sergio L C; Vale, Maria Goreti R; Welz, Bernhard

    2013-01-01

    A simple method has been developed to determine antimony and lead in pewter alloy cups produced in Brazil, using fast sequential determination by high-resolution continuum source flame atomic absorption spectrometry. The samples were dissolved in HCl and H(2)O(2), employing a cold finger system in order to avoid analyte losses. The main resonance line of lead at 217.001 nm and a secondary line of antimony at 212.739 nm were used. The limits of detection for lead and antimony were 0.02 and 5.7 mg L(-1), respectively. The trueness of the method was established by recovery tests and comparing the results obtained by the proposed method with those obtained by inductively coupled plasma optical emission spectrometry. The results were compared using a student's t-test and there was no significant difference at a 95% confidence interval. With the developed methods, it was possible to determine accurately antimony and lead in pewter samples. The lead concentration found in the analysed samples was around 1 mg g(-1), which means that they are not lead free; however, the content was below the maximum allowed level of 5 mg g(-1). The antimony content, which was found to be between 40 and 46 mg g(-1), is actually of greater concern, as antimony is known to be potentially toxic already at very low concentrations, although there is no legislation yet for this element.

  2. Quantification of absorption, retention and elimination of two different oral doses of vitamin A in Zambian boys using accelerator mass spectrometry

    SciTech Connect

    Aklamati, E K; Mulenga, M; Dueker, S R; Buchholz, B A; Peerson, J M; Kafwembe, E; Brown, K H; Haskell, M J

    2009-10-12

    A recent survey indicated that high-dose vitamin A supplements (HD-VAS) had no apparent effect on vitamin A (VA) status of Zambian children <5 y of age. To explore possible reasons for the lack of response to HD-VAS among Zambian children, we quantified the absorption, retention, and urinary elimination of either a single HDVAS (60 mg) or a smaller dose of stable isotope (SI)-labeled VA (5 mg), which was used to estimate VA pool size, in 3-4 y old Zambian boys (n = 4 for each VA dose). A 25 nCi tracer dose of [{sup 14}C{sub 2}]-labeled VA was co-administered with the HD-VAS or SI-labeled VA, and 24-hr stool and urine samples were collected for 3 and 7 consecutive days, respectively, and 24-hr urine samples at 4 later time points. Accelerator Mass Spectrometry (AMS) was used to measure the cumulative excretion of {sup 14}C in stool and urine 3d after dosing to estimate, respectively, absorption and retention of the VAS and SI-labeled VA. The urinary elimination rate (UER) was estimated by plotting {sup 14}C in urine vs. time, and fitting an exponential equation to the data. Estimates of mean absorption, retention and the UER were 83.8 {+-} 7.1%, 76.3 {+-} 6.7%, and 1.9 {+-} 0.6%/d, respectively, for the HD-VAS and 76.5 {+-} 9.5%, 71.1 {+-} 9.4%, and 1.8 {+-} 1.2%/d, respectively for the smaller dose of SI-labeled VA. Estimates of absorption, retention and the UER did not differ by size of the VA dose administered (P=0.26, 0.40, 0.88, respectively). Estimated absorption and retention were negatively associated with reported fever (P=0.011) and malaria (P =0.010). HD-VAS and SI-labeled VA were adequately absorbed, retained and utilized in apparently healthy Zambian preschool-age boys, although absorption and retention may be affected by recent infections.

  3. A reduced-scale railway noise barrier's insertion loss and absorption coefficients: comparison of field measurements and predictions

    NASA Astrophysics Data System (ADS)

    Busch, T. A.; Nugent, R. E.

    2003-10-01

    In situ testing determined the insertion loss ( IL) and absorption coefficients of a candidate absorptive noise barrier (soundwall) to abate railway noise for residents of Anaheim, CA. A 4000 m barrier is proposed south of the tracks, but residential areas to the north have expressed concerns that barrier reflections will increase their noise exposure. To address these concerns, a 3.66 m high by 14.6 m long demonstration barrier was built in the parking lot of Edison Field, Anaheim, as part of a public open house, thereby allowing for acoustical measurements. Insertion loss ( IL) was measured in third-octave bands assuming 1/2-scale construction. The IL for three, scaled railway noise sub-sources (rail/wheel interface, locomotive, and train horn) was measured at six, scaled distances. The highest total, A-weighted IL, after corrections for finite-barrier and point-source speaker effects was 22 dB(A) for rail/wheel noise, 18 dB(A) for locomotive noise, and 20 dB(A) for train horn noise. These results can be compared favourably to IL predictions made using algorithms from the US Federal Rail Administration (FRA) noise assessment guidelines. For the actual barrier installation, shielded residential receivers located south of the project are expected to see their future noise exposures reduced from an unmitigated 78 CNEL to 65 CNEL. Absorption coefficients were measured using time delay spectrometry. At lower frequencies, measured absorption coefficients were notably less than the reverberation room results advertised in the manufacturer's literature, but generally conformed with impedance tube results. At higher frequencies the correspondence between measured absorption coefficients and reverberation room results was much improved. For the actual barrier installation, unshielded residential receivers to the north are expected to experience noise exposure increases of less than 1 dB(A). This factor of increase is consistent with a finding of no impact when assessed

  4. [Determination of trace silver in water samples by solid phase extraction portable tungsten-coil electrothermal atomic absorption spectrometry].

    PubMed

    Fan, Guang-yu; Jiang, Xiao-ming; Zheng, Cheng-bin; Hou, Xian-deng; Xu, Kai-lai

    2011-07-01

    A simple method has been developed for the determination of silver in environmental water samples using solid phase extraction with tungsten-coil electrothermal atomic absorption spectrometry. Silica gel was used as an adsorbent and packed into a syringe barrel for solid phase extraction of silver prior to its determination by using a portable tungsten-coil electrothermal atomic absorption spectrometer. Optimum conditions for adsorption and desorption of silver ion, as well as interferences from co-existing ions, were investigated. A sample pH value of 6.0, a sample loading flow rate of 4.0 mL x min(-1), and the mixture of 4% (m/v) thiourea and 2% (phi) nitrate acid with the eluent flow rate of 0.5 mL x min(-1) for desorption were selected for further studies. Under optimal conditions, a linear range of 0.20-4.00 ng x mL(-1), a limit of detection (3sigma) of 0.03 ng x mL(-1) and a preconcentration factor of 94 were achieved. The proposed method was validated by testing three environmental water samples with satisfactory results.

  5. Determination of trace concentrations of chlorine in aqueous solutions by high-resolution continuum source graphite furnace molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Machyňák, Ľubomír; Čacho, František; Němeček, Martin; Beinrohr, Ernest

    2016-11-01

    Trace concentrations of total chlorine were determined by means of molecular absorption of indium mono-chloride (InCl) at 267.217 nm using high-resolution continuum source graphite furnace molecular absorption spectrometry. The effects of chemical modifiers and the amount of In on the sensitivity and accuracy were investigated. The optimum pyrolysis and vaporization temperatures were 600 °C and 1400 °C, respectively. The limit of detection and characteristic mass were found to be 0.10 ng and 0.21 ng, respectively. Potential non-spectral and spectral interferences were tested for various metals and non-metals at concentrations up to 50 mg L- 1 and for phosphoric, sulphuric and nitric acids. No spectral interferences were observed. Significant non-spectral interferences were observed with F, Br, and I at concentrations higher than 1 mg L- 1, 5 mg L- 1 and 25 mg L- 1, respectively, which is probably caused by formation of competitive indium halogen molecules. Higher concentrations of mineral acids depressed the signal owing to the formation of volatile HCl. The calibration curve was linear in the range between 0.3 and 10 ng with a correlation coefficient of R = 0.993. The elaborated method was used for the chlorine determination in various waters and a drug sample.

  6. A simple indirect automatic method to determine total iodine in milk products by flame atomic absorption spectrometry.

    PubMed

    Yebra, M C; Bollaín, M H

    2010-07-15

    A simple, precise and accurate automatic method for the determination of total iodine in milk products by indirect atomic absorption spectrometry is proposed. Iodide in solutions resulting from alkaline ashing of samples is precipitated with silver ion in a precipitation-dissolution flow manifold, which allows performing on-line the retention of the silver iodide precipitate formed on a filter, its wash with diluted ammonia and its dissolution with a diluted thiosulfate solution. Dissolved silver is also determined on-line by flame atomic absorption, and the achieved amount of this metal is proportional to that of iodine in the sample. The proposed method is very selective, avoids interferences from anions present in the samples, which can be also precipitated with silver, because these silver compounds are dissolved with ammonia at the washing step. This method allows the determination of iodine in the range 0.011-0.35 microg mL(-1) with a relative standard deviation between 1.3 and 6.8% at a rate of ca. 17 samplesh(-1).

  7. Determination of mercury in airborne particulate matter collected on glass fiber filters using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling

    NASA Astrophysics Data System (ADS)

    Araujo, Rennan G. O.; Vignola, Fabíola; Castilho, Ivan N. B.; Borges, Daniel L. G.; Welz, Bernhard; Vale, Maria Goreti R.; Smichowski, Patricia; Ferreira, Sérgio L. C.; Becker-Ross, Helmut

    2011-05-01

    A study has been undertaken to assess the capability of high-resolution continuum source graphite furnace atomic absorption spectrometry for the determination of mercury in airborne particulate matter (APM) collected on glass fiber filters using direct solid sampling. The main Hg absorption line at 253.652 nm was used for all determinations. The certified reference material NIST SRM 1648 (Urban Particulate Matter) was used to check the accuracy of the method, and good agreement was obtained between published and determined values. The characteristic mass was 22 pg Hg. The limit of detection (3σ), based on ten atomizations of an unexposed filter, was 40 ng g - 1 , corresponding to 0.12 ng m - 3 in the air for a typical air volume of 1440 m 3 collected within 24 h. The limit of quantification was 150 ng g -1, equivalent to 0.41 ng m -3 in the air. The repeatability of measurements was better than 17% RSD (n = 5). Mercury concentrations found in filter samples loaded with APM collected in Buenos Aires, Argentina, were between < 40 ng g -1 and 381 ± 24 ng g -1. These values correspond to a mercury concentration in the air between < 0.12 ng m -3 and 1.47 ± 0.09 ng m -3. The proposed procedure was found to be simple, fast and reliable, and suitable as a screening procedure for the determination of mercury in APM samples.

  8. Determination of phospholipids in soybean lecithin samples via the phosphorus monoxide molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry.

    PubMed

    Pires, Laís N; Brandão, Geovani C; Teixeira, Leonardo S G

    2017-06-15

    This paper presents a method for determining phospholipids in soybean lecithin samples by phosphorus determination using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) via molecular absorption of phosphorus monoxide. Samples were diluted in methyl isobutyl ketone. The best conditions were found to be 213.561nm with a pyrolysis temperature of 1300°C, a volatilization temperature of 2300°C and Mg as a chemical modifier. To increase the analytical sensitivity, measurement of the absorbance signal was obtained by summing molecular transition lines for PO surrounding 213nm: 213.561, 213.526, 213.617 and 213.637nm. The limit of detection was 2.35mgg(-1) and the precision, evaluated as relative standard deviation (RSD), was 2.47% (n=10) for a sample containing 2.2% (w/v) phosphorus. The developed method was applied for the analysis of commercial samples of soybean lecithin. The determined concentrations of phospholipids in the samples varied between 38.1 and 45% (w/v).

  9. Synthesis of a new molecularly imprinted polymer for sorption of the silver ions from geological and antiseptic samples for determination by flame atomic absorption spectrometry.

    PubMed

    Hashemi-Moghaddam, Hamid; Yahyazadeh, Faegheh; Vardini, Mohammad Taghi

    2014-01-01

    A new molecularly imprinted polymer (MIP) was synthesized using methacrylic acid (functional monomer), ethylene glycol dimethacrylate (crosslinker), 2,2'-azobisisobutironitril (initiator), silver (Ag) dithizone complex (template), and chloroform (porogenic solvent). This process was a noncovalent, bulk, thermal radical-polymerization. To compare the performance of this polymer, control polymer (nonimprinted polymer) was prepared under well-defined conditions without the use of a template. Extraction experiments were performed on the MIP and a nonimprinted polymer. Then, various parameters were optimized, such as pH, time, concentration of sample, and type of eluent for elution of Ag from polymer. In addition, interfering effects were investigated on the absorption of Ag by the MIP. This polymer was used for the rapid extraction and preconcentration of Ag from an antiseptic and geological sample. Finally, the amount of Ag was measured by flame atomic absorption spectrometry after preconcentration by the synthesized MIP, and results were compared with a direct inductively coupled plasma method. The results showed high performance of this method in preconcentration of Ag.

  10. Improved self-absorption correction for extended x-ray absorption fine-structure measurements

    SciTech Connect

    Booth, C.H.; Bridges, F.

    2003-06-04

    Extended x-ray absorption fine-structure (EXAFS) data collected in the fluorescence mode are susceptible to an apparent amplitude reduction due to the self-absorption of the fluorescing photon by the sample before it reaches a detector. Previous treatments have made the simplifying assumption that the effect of the EXAFS on the correction term is negligible, and that the samples are in the thick limit. We present a nearly exact treatment that can be applied for any sample thickness or concentration, and retains the EXAFS oscillations in the correction term.

  11. Determination of sulphur in various vegetables by solid sampling high-resolution electrothermal molecular absorption spectrometry.

    PubMed

    Gunduz, Sema; Akman, Suleyman

    2015-04-01

    Sulphur was determined in various vegetables via molecular absorption of carbon monosulphide (CS) at 258.056 nm using a solid sampling high resolution continuum source electrothermal atomic absorption spectrometer (SS HR-CS ETAAS). Samples were dried, ground and directly introduced into the ruthenium coated graphite furnace as 0.05 to 0.50mg. All determinations were performed using palladium+citric acid modifier and applying a pyrolysis temperature of 1000 °C and a volatilisation temperature of 2400 °C. The results were in good agreement with certified sulphur concentrations of various vegetal CRM samples applying linear calibration technique prepared from thioacetamide. The limit of detection and characteristic mass of the method were 7.5 and 8.7 ng of S, respectively. The concentrations of S in various spinach, leek, lettuce, radish, Brussels sprouts, zucchini and chard samples were determined. It was showed that distribution of sulphur in CRM and grinded food samples were homogeneous even in micro-scale.

  12. In situ Gas Temperature Measurements by UV-Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fateev, A.; Clausen, S.

    2009-02-01

    The absorption spectrum of the NO A2Σ+ ← X2Πγ-system can be used for in situ evaluation of gas temperature. Experiments were performed with a newly developed atmospheric-pressure high-temperature flow gas cell at highly uniform and stable gas temperatures over a 0.533 m path in the range from 23 °C to 1,500 °C. The gas temperature was evaluated (1) from the analysis of the structure of selected NO high-resolution γ-absorption bands and (2) from the analysis of vibrational distribution in the NO γ-absorption system in the (211-238) nm spectral range. The accuracy of both methods is discussed. Validation of the classical Lambert-Beer law has been demonstrated at NO concentrations up to 500 ppm and gas temperatures up to 1,500 °C over an optical absorption path length of 0.533 m.

  13. Improving accuracy in the quantitation of overlapping, asymmetric, chromatographie peaks by deconvolution: theory and application to coupled gas chromatography atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Johansson, M.; Berglund, M.; Baxter, D. C.

    1993-09-01

    Systematic errors in the measurement of overlapping asymmetric, Chromatographic peaks are observed using the perpendicular-drop and tangent-skimming algorithms incorporated in commercial integrators. The magnitude of such errors increases with the degree of tailing and differences in peak size, and was found to be as great as 80% for peak-area and 100% for peak-height measurements made on the smaller, second component of simulated, noise-free chromatograms containing peaks at a size ratio of 10 to 1. Initial deconvolution of overlapping peaks, by mathematical correction for asymmetry, leads to significant improvements in the accuracy of both peak-area and height measurements using the simple, perpendicular-drop algorithm. A comparison of analytical data for the separation and determination of three organolead species by coupled gas chromatography atomic absorption spectrometry using peak-height and area measurements also demonstrates the improved accuracy obtained following deconvolution. It is concluded that the deconvolution method described could be beneficial in a variety of Chromatographic applications where overlapping, asymmetric peaks are observed.

  14. Geodetic Mobile Solar Spectrometry: Description of the New Spectrometer GEMOSS and First Measurements

    NASA Astrophysics Data System (ADS)

    Somieski, A.; Buerki, B.; Kahle, H.-G.; Becker-Ross, H.; Florek, S.; Okruss, M.

    2003-04-01

    In former scientific research projects of the Geodesy and Geodynamic Laboratory (GGL) the method of solar spectrometry has demonstrated its performance as a remote sensing technique for determination of integrated precipitable water vapor (IPWV). A first prototype, named Solar Atmospheric MOnitoring Spectrometer (SAMOS), was developed at GGL in cooperation with the Institute of Spectrochemistry and Applied Spectroscopy (ISAS) in Berlin. A new type of solar spectrometer for geodetic applications is currently under development. In this project the construction of the first prototype GEMOSS I (Geodetic MObile Solar Spectrometer) has been completed. It provides simultaneous measurements of water vapor absorption lines in the range from 730 nm to 910 nm with a spectral resolution of 10-15 pm. This technique allows a compact design, low weight as well as high time resolution and accuracy of IPWV at a relatively low level of costs. First measurements were carried out to verify the system stability under field conditions and the data quality. The presentation will highlight the technical innovations of GEMOSS I and will show results of first measurements.

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

    USGS Publications Warehouse

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

    1976-01-01

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

  16. Determination of tributyltin in tissues and sediments by graphite furnace atomic absorption spectrometry

    SciTech Connect

    Stephenson, M.D.; Smith, D.R.

    1988-04-01

    A method for the determination of tributyltin (TBT) in tissue and sediments has been developed for environmental samples. The technique involves extraction with methylene chloride and isolation of TBT from mono- and dibutyltin with a sodium hydroxide wash. The TBT is then back extracted and converted to elemental Sn with nitric acid. Analysis is by Zeeman graphite furnace atomic absorption spectrophotometry. Recoveries of spiked samples were between 99% and 111% for mussel and fish tissues and 72% and 99% for various sediments. The limit of quantification was 0.0025 ..mu..g/g for tissue (on a wet weight basis). This technique was developed in response to their need to process large numbers of environmental samples with a minimum time investment.

  17. Comparison of different sample preparation methods for platinum determination in cultured cells by graphite furnace atomic absorption spectrometry

    PubMed Central

    Cai, Jing; Jia, Jinghui; Zhang, Yuzeng; Dong, Weihong

    2017-01-01

    Background Platinum-based agents are widely used in chemotherapy against solid tumors and insufficient intracellular drug accumulation is one of the leading causes of platinum resistance which is associated with poor survival of tumor patients. Thus, the detection of intracellular platinum is pivotal for studies aiming to overcome platinum resistance. In the present study, we aimed to establish a reliable graphite furnace atomic absorption spectrometry (GFAAS)-based assay to quantify the intracellular platinum content for cultured cells. Methods Several most commonly applied cell preparation methods, including 0.2% HNO3, 0.2% Triton X-100, concentrated nitric acid, RIPA combined with concentrated nitric acid and hydroxide, followed by GFAAS for platinum detection were compared in ovarian, cervical and liver cancer cell lines to obtain the optimal one, and parameters regarding linearity, accuracy, precision and sensitivity were evaluated. Influence of other metals on platinum detection and the storage conditions of samples were also determined. Results The treatment of cells with 0.2% HNO3 was superior to other approaches with fewer platinum loss and better repeatability. The recovery rate and precision of this method were 97.3%–103.0% and 1.4%–3.8%, respectively. The average recoveries in the presence of other metals were 95.1%–103.1%. The detection limit was 13.23 ug/L. The recovery rate of platinum remained acceptable even in cell samples stored in −20 °C or −80 °C for two months. Discussion After comparison, we found that 0.2% HNO3 was optimal for intracellular platinum quantification based on GFAAS, which presented values compatible with that of inductively-coupled plasma mass-spectrometry (ICP-MS), and this is partially attributed to the simplicity of this method. Moreover, the assay was proved to be accurate, sensitive, cost-effective and suitable for the research of platinum-based antitumor therapy. PMID:28123908

  18. Advances in Methane Isotope Measurements via Direct Absorption Spectroscopy with Applications to Oil and Gas Source Characterization

    NASA Astrophysics Data System (ADS)

    Yacovitch, T. I.; Herndon, S. C.; Roscioli, J. R.; Petron, G.; Shorter, J. H.; Jervis, D.; McManus, J. B.; Nelson, D. D.; Zahniser, M. S.; Kolb, C. E., Jr.

    2015-12-01

    Instrumental developments in the measurement of multiple isotopes of methane (12CH4, 13CH4 and 12CH3D) are presented. A first generation 8-micron instrument quantifies 12CH4 and 13CH4 at a 1-second rate via tunable infrared direct absorption spectroscopy (TILDAS). A second generation instrument uses two 3-micron intraband cascade lasers in an Aerodyne dual laser chassis for simultaneous measurement of 12CH4, 13CH4 and 12CH3D. Sensitivity and noise performance improvements are examined. The isotopic signature of methane provides valuable information for emission source identification of this greenhouse gas. A first generation spectrometer has been deployed in the field on a mobile laboratory along with a sophisticated 4-tank calibration system. Calibrations are done on an agressive schedule, allowing for the correction of measured isotope ratios to an absolute isotope scale. Distinct isotopic signatures are found for a number of emission sources in the Denver-Julesburg Basin: oil and gas gathering stations, compressor stations and processing plants; a municipal landfill, and dairy/cattle operations. The isotopic signatures are compared with measured ethane/methane ratios. These direct absorption measurements have larger uncertainties than samples measured via gas chromatography-mass spectrometry, but have several advantages over canister sampling methods: individual sources of short duration are easier to isolate; calibrated isotope ratio results are available immediately; replicate measurements on a single source are easily performed; and the number of sources sampled is not limited by canister availability and processing time.

  19. Germanium determination by flame atomic absorption spectrometry: an increased vapor pressure-chloride generation system.

    PubMed

    Kaya, Murat; Volkan, Mürvet

    2011-03-15

    A new chloride generation system was designed for the direct, sensitive, rapid and accurate determination of the total germanium in complex matrices. It was aimed to improve the detection limit of chloride generation technique by increasing the vapor pressure of germanium tetrachloride (GeCl(4)). In order to do so, a novel joint vapor production and gas-liquid separation unit equipped with a home-made oven was incorporated to an ordinary nitrous oxide-acetylene flame atomic absorption spectrometer. Several variables such as reaction time, temperature and acid concentration have been investigated. The linear range for germanium determination was 0.1-10 ng mL(-1) for 1 mL sampling volume with a detection limit (3s) of 0.01 ng mL(-1). The relative standard deviation (RSD) was 2.4% for nine replicates of a 1 ng mL(-1) germanium solution. The method was validated by the analysis of one non-certified and two certified geochemical reference materials, respectively, CRM GSJ-JR-2 (Rhyolite), and GSJ-JR-1 (Rhyolite), and GBW 07107 (Chinese Rock). Selectivity of the method was investigated for Cd(2+), Co(2+), Cu(2+), Fe(3+), Ga(3+), Hg(2+), Ni(2+), Pb(2+), Sn(2+), and Zn(2+) ions and ionic species of As(III), Sb(III), Te(IV), and Se(IV).

  20. Determination of fluorine in milk samples via calcium-monofluoride by electrothermal molecular absorption spectrometry.

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2013-05-01

    The determination of fluorine in milk samples via the molecular absorption of calcium mono-fluoride (CaF) was performed using a HR-CS-ETAAS. For this purpose, calcium was pipetted to graphite furnace together with samples. The amount of Ca and the graphite furnace program were optimised. Fluorine was determined in pyrolytically coated platforms at 606.440 nm applying a pyrolysis temperature of 700 °C and a molecule forming temperature of 2250 °C. Finally, applying standard addition technique, F contents of several milk samples were determined. The results obtained by linear calibration and standard addition techniques were significantly different which can be attributed to non-spectral interferences in milk due to matrix concomitants. Therefore, in order to tolerate the errors, the F contents of several milk samples were determined applying standard addition technique. However, since the ingredients of milk samples change for different kinds, the F in each sample was determined from its own standard addition curve. The range of F content for the milk samples were 0.027-0.543 μg mL(-1). The limit of detection and characteristic mass of the method were 0.26 and 0.13 ng of F, respectively.

  1. Determination of mercury(II) ion by electrochemical cold vapor generation atomic absorption spectrometry.

    PubMed

    Arbab-Zavar, M Hosein; Rounaghi, G Hosein; Chamsaz, Mahmoud; Masrournia, Mahboube

    2003-05-01

    A technique for determination of mercury is described; it is based on electrolytic reduction of Hg(II) ion on a graphite cathode, the trapping of mercury vapor and its volatilization into a quartz tube aligned in the optical path of an atomic absorption spectrometer. The electrochemical cell consisted of a graphite cathode and an anode operating with constant direct current for the production of mercury atoms. A pre-activated graphite rod was used as the cathode material. The optimum conditions for electrochemical generation of mercury cold vapor (the electrolysis time and current, the flow rate, the type of electrode and electrolyte) were investigated. The characteristic electrochemical data with chemical cold vapor using NaBH4-acid were compared. The presence of cadmium(II), arsenic(III), antimony(III), selenium(IV), bismuth(III), silver(I), lead(II), lithium(I), sodium(I) and potassium(I) showed interference effects which were eliminated by suitable separation techniques. The calibration curve is linear over the range of 5-90 ng ml(-1) mercury(II). The detection limit is 2 ng ml(-1) of Hg(II) and the RSD is 2.5% (n = 10) for 40 ng ml(-1). The accuracy and recovery of the method were investigated by analyzing spiked tap water and river water.

  2. Direct determination of fluorine in niobium oxide using slurry sampling electrothermal high-resolution continuum source molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Huang, Mao Dong; Becker-Ross, Helmut; Okruss, Michael; Geisler, Sebastian; Florek, Stefan; Richter, Silke; Meckelburg, Angela

    Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H2SO4, and H3PO4. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes.

  3. Measurements of the Absorption by Auditorium SEATING—A Model Study

    NASA Astrophysics Data System (ADS)

    BARRON, M.; COLEMAN, S.

    2001-01-01

    One of several problems with seat absorption is that only small numbers of seats can be tested in standard reverberation chambers. One method proposed for reverberation chamber measurements involves extrapolation when the absorption coefficient results are applied to actual auditoria. Model seat measurements in an effectively large model reverberation chamber have allowed the validity of this extrapolation to be checked. The alternative barrier method for reverberation chamber measurements was also tested and the two methods were compared. The effect on the absorption of row-row spacing as well as absorption by small numbers of seating rows was also investigated with model seats.

  4. On the errors in measuring the particle density by the light absorption method

    SciTech Connect

    Ochkin, V. N.

    2015-04-15

    The accuracy of absorption measurements of the density of particles in a given quantum state as a function of the light absorption coefficient is analyzed. Errors caused by the finite accuracy in measuring the intensity of the light passing through a medium in the presence of different types of noise in the recorded signal are considered. Optimal values of the absorption coefficient and the factors capable of multiplying errors when deviating from these values are determined.

  5. Inference of the microwave absorption coefficient from stray radiation measurements in Wendelstein 7-X

    NASA Astrophysics Data System (ADS)

    Moseev, D.; Laqua, H. P.; Marsen, S.; Marushchenko, N.; Stange, T.; Braune, H.; Gellert, F.; Hirsch, M.; Hoefel, U.; Knauer, J.; Oosterbeek, J. W.; Turkin, Y.; The Wendelstein 7-X Team

    2017-03-01

    The efficiency of electron cyclotron heating is determined by the microwave absorption of the plasma. Good microwave absorption is also crucial for the machine safety. In this paper we present a method of evaluating the microwave absorption coefficient from stray radiation measurements. The discussed method is computationally simple and can be applied potentially in real time. Evolution of the second harmonic extraordinary mode (X2) microwave absorption coefficient in Wendelstein 7-X during the start-up phase is presented, as well as an estimate of the absorption coefficient for the second harmonic ordinary mode (O2) wave.

  6. Determination of cadmium in coal using solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry.

    PubMed

    da Silva, Alessandra Furtado; Borges, Daniel L G; Lepri, Fábio Grandis; Welz, Bernhard; Curtius, Adilson J; Heitmann, Uwe

    2005-08-01

    This work describes the development of a method to determine cadmium in coal, in which iridium is used as a permanent chemical modifier and calibration is performed against aqueous standards by high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). This new instrumental concept makes the whole spectral environment in the vicinity of the analytical line accessible, providing a lot more data than just the change in absorbance over time available from conventional instruments. The application of Ir (400 microg) as a permanent chemical modifier, thermally deposited on the pyrolytic graphite platform surface, allowed pyrolysis temperatures of 700 degrees C to be used, which was sufficiently high to significantly reduce the continuous background that occurred before the analyte signal at pyrolysis temperatures <700 degrees C. Structured background absorption also occurred after the analyte signal when atomization temperatures of >1600 degrees C were used, which arose from the electron-excitation spectrum (with rotational fine structure) of a diatomic molecule. Under optimized conditions (pyrolysis at 700 degrees C and atomization at 1500 degrees C), interference-free determination of cadmium in seven certified coal reference materials and two real samples was achieved by direct solid sampling and calibrating against aqueous standards, resulting in good agreement with the certified values (where available) at the 95% confidence level. A characteristic mass of 0.4 pg and a detection limit of 2 ng g(-1), calculated for a sample mass of 1.0 mg coal, was obtained. A precision (expressed as the relative standard deviation, RSD) of <10% was typically obtained when coal samples in the mass range 0.6-1.2 mg were analyzed.

  7. Determination of selected elements in whole coal and in coal ash from the eight argonne premium coal samples by atomic absorption spectrometry, atomic emission spectrometry, and ion-selective electrode

    USGS Publications Warehouse

    Doughten, M.W.; Gillison, J.R.

    1990-01-01

    Methods for the determination of 24 elements in whole coal and coal ash by inductively coupled argon plasma-atomic emission spectrometry, flame, graphite furnace, and cold vapor atomic absorption spectrometry, and by ion-selective electrode are described. Coal ashes were analyzed in triplicate to determine the precision of the methods. Results of the analyses of NBS Standard Reference Materials 1633, 1633a, 1632a, and 1635 are reported. Accuracy of the methods is determined by comparison of the analysis of standard reference materials to their certified values as well as other values in the literature.

  8. DEVELOPMENT OF ULTRATRACE LASER SPECTROMETRY TECHNIQUES FOR MEASUREMENTS OF ARSENIC

    EPA Science Inventory


    Development of Arsenic Speciation Techniques Based on High Performance Liquid Chromatography and Atomic Fluorescence Spectrometry

    J.B. Simeonsson, H.D. Beach and D.J. Thomas
    US EPA, Office of Research and Development, National Health and Environmental Effects Resear...

  9. Acoustic Absorption Measurements for Characterization of Gas Mixing

    DTIC Science & Technology

    2007-11-02

    of the box (Gas A). Gas B is humidified by passing the same grade CO2 through a bubbler. The humidity of the gas is varied by mixing the relative...the accuracy with which the “mixedness profile” can be inverted. 1Bhatia, A., Ultrasonic Absorption, Dover Publications: New York, 1967. 2

  10. Measurement of the 135Cs half-life with accelerator mass spectrometry and inductively coupled plasma mass spectrometry

    NASA Astrophysics Data System (ADS)

    MacDonald, C. M.; Cornett, R. J.; Charles, C. R. J.; Zhao, X. L.; Kieser, W. E.

    2016-01-01

    The isotope 135Cs is quoted as having a half-life of 2.3 Myr. However, there are three published values ranging from 1.8 to 3 Myr. This research reviews previous measurements and reports a new measurement of the half-life using newly developed accelerator mass spectrometry (AMS) and inductively coupled plasma mass spectrometry (ICPMS) techniques along with β and γ radiometric analysis. The half-life was determined to be (1.6 ±0.6 ) ×106 yr by AMS and (1.3 ±0.2 ) ×106 yr by ICPMS with 95% confidence. The two values agree with each other but differ from the accepted value by ˜40 % .

  11. Determination of trace amounts of molybdenum in plant tissue by solvent extraction-atomic-absorption and direct-current plasma emission spectrometry.

    PubMed

    Lajunen, L H; Kubin, A

    1986-03-01

    Methods are presented for determination of molybdenum in plant tissue by flame and graphite-furnace atomic-absorption spectrometry and direct-current argon-plasma emission spectrometry. The samples are digested in HNO(3)-H(2)SO(4)-HC1O(4) mixture, and Mo is separated and concentrated by chelation and extraction. Three organic solvents (methyl isobutyl ketone, di-isobutyl ketone and isoamyl alcohol) and two ligands (8-hydroxyquinoline and toluene-3,4-dithiol) were studied. The procedure were tested on pine needle and birch leaf samples.

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

    NASA Technical Reports Server (NTRS)

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

    2013-01-01

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

  13. Determination of trace amounts of zinc by flame atomic absorption spectrometry after preconcentration with modified clinoptilolite zeolite.

    PubMed

    Hajialigol, Saeed; Taher, Mohammad Ali; Malekpour, Akbar

    2008-01-01

    Natural clinoptilolite was used as a sorbent material for solid-phase extraction and preconcentration of zinc. Clinoptilolite was first saturated with cadmium (II) and then modified with benzyldimethyltetradecylammonium chloride for increasing adsorption of 3-(2-arsenophenylazo)-4,5-dihydroxy-2,7-naphthalene disulfonic acid (neothorin). Zinc was quantitatively retained on the adsorbent by the column method in the pH range of 3.8-4.2 at a flow rate of 1 mL/min. It was eluted from the column with 5.0 mL 2 M nitric acid solution at a flow rate of 1 mL/min and determined by flame atomic absorption spectrometry at 213.9 nm. Zinc could be concentrated from a 0.03 microg/L solution with a preconcentration factor of 170. Relative standard deviation for 8 replicate determinations of 2.5 microg zinc in the final solution was 0.92%. The interference of a large number of anions and cations was studied in detail to optimize the conditions, and the method was successfully applied for determination of zinc in standard and real water samples.

  14. Calcium in the developing Ambystoma neural axis shown by 3H and fluorescent chlortetracycline and atomic absorption spectrometry

    SciTech Connect

    Moran, D.J. )

    1990-12-01

    The calcium ion has been implicated in the mediation of the morphogenetic movements that occur during neural tube formation. The present study identifies high levels of calcium in the neuroepithelium of the neural plate, folds, and tube. These levels are substantially higher than those discerned elsewhere in the embryo. The calcium is localized in morphogenetically active regions by using the antibiotic chlortetracycline (CTC) which chelates calcium and is demonstrated in this investigation by both autoradiography and calcium-linked fluorescence. The specificity of CTC reaction for calcium in the developing neural axis is confirmed by EGTA competition. A comparison of the actual calcium levels in the developing neural axis (dorsal) with equivalently weighted ventral tissues was obtained by atomic absorption spectrometry (AAS). This method provides a total count of the calcium without any loss during tissue processing. For AAS, living tissues were precisely excised and immediately dessicated. Each tissue sample (dry weight 1.5 mg) was then solubilized for analysis. The spectrometric data reveal that the embryonic dorsal aspect forming the neural tube contains 57% more calcium than an equivalent weight of the ventral aspect.

  15. Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

    PubMed

    Feichtmeier, Nadine S; Leopold, Kerstin

    2014-06-01

    In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples.

  16. Selective speciation of inorganic antimony on tetraethylenepentamine bonded silica gel column and its determination by graphite furnace atomic absorption spectrometry.

    PubMed

    Mendil, Durali; Bardak, Hilmi; Tuzen, Mustafa; Soylak, Mustafa

    2013-03-30

    A speciation system for antimony (III) and antimony (V) ions that based on solid phase extraction on tetraethylenepentamine bonded silica gel has been established. Antimony was determined by graphite furnace atomic absorption spectrometry (GF-AAS). Analytical conditions including pH, sample volume, etc., were studied for the quantitative recoveries of Sb (III) and Sb (V). Matrix effects on the recovery were also investigated. The recovery values and detection limit for antimony (III) at optimal conditions were found as >95% and 0.020 μg L(-1), respectively. Preconcentration factor was calculated as 50. The capacity of adsorption for the tetraethylenepentamine bonded silica gel was 7.9 mg g(-1). The validation was checked by analysis of NIST SRM 1573a Tomato laves and GBW 07605 Tea certified reference materials. The procedure was successfully applied to speciation of antimony in tap water, mineral water and spring water samples. Total antimony was determined in refined salt, unrefined salt, black tea, rice, tuna fish and soil samples after microwave digestion and presented enrichment method combination.

  17. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry.

    PubMed

    Ghaedi, M; Shokrollahi, A; Ahmadi, F; Rajabi, H R; Soylak, M

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L(-1) HNO(3) nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO(3), bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL(-1) for Cu(2+), Co(2+) and Ni(2+) along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu(2+), Ni(2+) and Co(2+), respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

  18. Analysis of metals in marine sediments by microwave extraction and flame, hydride generation and cold vapor atomic-absorption spectrometry

    SciTech Connect

    Martinez-Garcia, M.L.; Zubieta, A.C.; Lorenzo, S.M.; Lopez-Mahia, P.; Rodriguez, D.P.

    1999-01-01

    A simple and fast metal extraction method that combines closed vessels and microwave heating for the simultaneous extraction of ten selected heavy metals (As, Cd, Co, Cr, Hg, Mn, Ni, Pb, Zn) from marine sediments is proposed. Digestion conditions, i.e., power and times microwave irradiation, reagent extractant, sample amount, were optimized to recover the potentially available metallic fraction not bound in silicates. A nitric acid and two step microwave program was established. The resulting solutions were analyzed by flame (FAAS), hydride generation (HG-AAS) and cold vapor (CV-AAS) atomic absorption spectrometry. Quantifications were made using direct calibration with aqueous standards. The recoveries of the spiked samples investigated ranged from 89 to 113%. The results obtained from analyzing the BCR certified reference sediment CRM 277 Estuarine Sediment were in good agreement with the certified values (93--105%), except for low values for chromium (79%). The relative standard deviations for the determination of metals were less than 4%. Finally, the technique designed herein was applied to sediment samples from La Coruna estuary, NW Spain.

  19. Comparison of two digestion procedures for the determination of lead in lichens by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Moreira, Fátima R.; Borges, Renato M.; Oliveira, Rosália M.

    2005-06-01

    The efficiency of two procedures for the digestion of lichen was investigated using a heating block and a microwave oven. In the open vessels, concentrated nitric acid was added to the samples, left for 1 h, and the addition of 30% (v / v) hydrogen peroxide completed the digestion. In the closed system, the complete digestion was performed using concentrated nitric acid and hydrogen peroxide, reducing the amount of chemicals, time and contamination risk. Both digestion methods gave comparable results, and recoveries were statistically not different. For a lichen sample spiked with 10 μg Pb, the recovery was 111% and 110% using microwave and heating block digestion, respectively, while it was 100% and 103% for a 100 μg Pb spike. For the determination by electrothermal atomic absorption spectrometry samples were diluted 20 times with water and a volume of 20 μL was injected into the graphite furnace without chemical modifier. Pyrolysis and atomization temperatures of 700 °C and 1500 °C, respectively, were used. The characteristic mass was 8.4 ± 0.6 pg for aqueous calibration solutions and 8.9 ± 0.8 pg for samples. Calibration was against matrix matched standards. The recovery test showed some contamination problem with the lowest concentrations in both procedures. The detection limits were 4.4 μg L - 1 with microwave oven and 5.4 μg L - 1 with the heating block in the undiluted blank.

  20. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    NASA Astrophysics Data System (ADS)

    Gil, Sandra; Fragueiro, Sandra; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium.

  1. Determination of Trace Silver in Water Samples by Online Column Preconcentration Flame Atomic Absorption Spectrometry Using Termite Digestion Product

    PubMed Central

    Bianchin, Joyce Nunes; Martendal, Edmar; Carasek, Eduardo

    2011-01-01

    A new method for Ag determination in water samples using solid phase extraction (SPE) coupled to a flow injection system and flame atomic absorption spectrometry was developed. The sorbent used for Ag preconcentration and extraction was the termite digestion product. Flow and chemical variables of the system were optimized through a multivariate procedure. The factors selected were adsorbent mass, buffer type and concentration, sample pH, and sample flow rate. The detection limit and precision were 3.4 μg L−1 and 3.8% (n = 6, 15 μg L−1), respectively. The enrichment factor and the linear working range were, respectively, 21 and 10–50 μg L−1. Results for recovery tests using different water samples were between 96 and 107%. The proposed methodology was applied with success for the determination of Ag in water used to wash clothes impregnated with silver nanoparticles, supplied by a factory located in Santa Catarina, Brazil. PMID:21804766

  2. Metal furnace heated by flame as a hydride atomizer for atomic absorption spectrometry: Sb determination in environmental and pharmaceutical samples.

    PubMed

    Figueiredo, Eduardo Costa; Dĕdina, Jirí; Arruda, Marco Aurélio Zezzi

    2007-10-15

    The present work describes a metallic hydride atomizer for atomic absorption spectrometry, by evaluating the performance of the Inconel 600((R)) tube. For this purpose, stibine was used as the model volatile compound and antimony determination in river and lake sediments and in pharmaceutical samples was carried out to assess the metal furnace performance. Some parameters are evaluated such as those referring to the generation and transport of the hydride (such as KBH(4) and acid concentrations, carrier gas flow rate, injected volume, etc.), as well as those referring to the metal furnace (such as tube hole area, flame composition, long-term stability, etc.). The method presents linear Sb concentration from 2 to 80mugL(-1) range (r>0.998; n=3) and the analytical frequency of ca. 140h(-1). The limit of detection (LOD) is 0.23mugL(-1) and the precision, expressed as R.S.D., is less than 5% (40mugL(-1); n=10). The accuracy is evaluated through the reference materials, and the results are similar at 95% confidence level according to the t-test.

  3. Determination of cadmium and lead in beverages after leaching from pewter cups using graphite furnace atomic absorption spectrometry.

    PubMed

    Dessuy, Morgana B; Vale, Maria Goreti R; Welz, Bernhard; Borges, Aline R; Silva, Márcia M; Martelli, Patrícia B

    2011-07-15

    Two simple methods have been developed to determine cadmium and lead in different kinds of beverages and vinegar leached from pewter cups produced in Brazil. Leaching experiments have been carried out with different solutions: beer, sugar cane spirit, red and white wine, vinegar and a 3% acetic acid solution. The solutions were kept in cups with and without solder for 24h. Lead and cadmium have been determined using graphite furnace atomic absorption spectrometry with deuterium background correction. The limits of detection were 0.05 and 1.4 μg L(-1), and the characteristic mass was 1.0 pg and 19 pg for Cd and Pb, respectively. With the developed methods it was possible to determine accurately cadmium and lead by direct analysis in these liquids and to evaluate the leaching of these metals from pewter cups. The results presented in this work show that pewter cups are not cadmium- and lead-free; this point goes against the manufacturers' declaration that their products are lead-free.

  4. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Woińska, Sylwia; Godlewska-Żyłkiewicz, Beata

    2011-07-01

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L - 1 thiourea in 0.3 mol L - 1 HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL - 1 for Pt and 0.012 ng mL - 1 for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g - 1 for Pt and 1.24 mg g - 1 for Pd.

  5. A new coupling of ionic liquid based-single drop microextraction with tungsten coil electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Wen, Xiaodong; Deng, Qingwen; Wang, Jiwei; Yang, Shengchun; Zhao, Xia

    2013-03-01

    In this work, an improved method of ionic liquid based-single drop microextraction (IL-SDME) preconcentration was firstly coupled with tungsten coil electrothermal atomic absorption spectrometry (W-coil ET-AAS) detection. The new coupling was developed and applied for the determination of ultra-trace cadmium. Experimental parameters influencing the performance of IL-SDME as well as instrumental conditions were studied systematically, including IL-drop volume, chelating agent concentration, pH, stirring rate and time, heating program of W-coil ET-AAS, flow rate of carrier gas. Under the optimal conditions, the limit of detection (LOD) for cadmium was 0.015 μg L-1 (sampling amount on W-coil was 10 μL). The sensitivity enhancement factor was 42, while the improvement factor of LOD was 33. The established method was applied to determine cadmium in standard reference materials of rice and real water samples successfully. The developed IL-SDME-W-coil ET-AAS coupling represents a simple, green and highly sensitive method for cadmium determination.

  6. Minimization of volatile nitrogen oxides interference in the determination of arsenic by hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    de Moraes Flores, Érico Marlon; da Silva, Letícia Longhi Cirne; Barin, Juliano Smanioto; Saidelles, Ana Paula Fleig; Zanella, Renato; Dressler, Valderi Luis; Paniz, José Neri Gottfried

    2001-10-01

    In this study emphasis was given to minimize the interference of volatile nitrogen oxides from digestion procedures with nitric acid on the determination of arsenic by hydride generation atomic absorption spectrometry (HG AAS). Sulfamic acid (SA) is proposed to minimize this interference by employing three procedures for the digestion of hair in closed systems: conventional and microwave (MW) heating in polytetrafluorethylene (PTFE) vessels and by MW heating in glass vials. Hair samples were digested with H 2SO 4+HNO 3 or HNO 3+H 2O 2 mixtures. Concentrated hydrochloric acid was added for the digestion for the procedure in glass vials. The accuracy of the procedures with PTFE vessels was verified by the spike recoveries of organic ( p-aminobenzenearsonic acid and dimethyl arsinic acid, from 92 to 101%) and inorganic (sodium arsenate, from 98 to 102%) arsenic compounds. For the procedure in glass vials the recovery was from 86 to 97% for organic As and from 97 to 102% for inorganic As. The results obtained for a certified hair reference material using the three digestion procedures were well within the 95% confidence interval of the certificate when SA was added to the solutions. However, when SA was not added, recoveries were low and non-reproducible signals and high background levels were observed. Urea, benzoic acid and hydroxylamine hydrochloride were also studied (maximum As recovery of 90% using hydroxylamine hydrochloride) but the best results were obtained with use of SA.

  7. Determination of tributyltin in toluene extract from sea water by graphite furnace atomic absorption spectrometry with a new matrix modifier.

    PubMed

    Gong, B; Liu, Y; Xu, Y; Lin, T

    1997-06-01

    A new matrix modifier composed of calcium and chromium[VI] was proposed for the determination of tributyltin (TBT) in toluene extract from sea water containing sediment by graphite furnace atomic absorption spectrometry (GFAAS). Fourteen inorganic and organic compounds (barium, calcium, chromium[VI], lanthanum, magnesium, nickel, palladium, strontium, calcium-chromium[VI], calcium-strontium, nickel isocaprylate, 5%-, 10%-aqueous solution of ascorbic acid and toluene-saturated solution of ascorbic acid) as a matrix modifier were comparatively studied and a matrix modifier composed from 5 microg of calcium and 1 microg of chromium[VI] was found to give the best performance. The interference effects of co-existing elements in sea water containing sediment (aluminium, iron, magnesium, sodium and strontium) were studied. TBT in eight toluene extracts was determined by GFAAS with the proposed matrix modifier. The relative standard deviation was 3.0% for 63 ng ml(-1) of TBT (n = 11). The recoveries were 88-104%. The characteristic mass was 7 pg. The linearity range was 0-250 ng mg(-1).

  8. Direct determination of Cu and Zn in fruit juices and bovine milk by thermospray flame furnace atomic absorption spectrometry.

    PubMed

    Nascentes, Clésia C; Arruda, Marco A Z; Nogueira, Ana Rita A; Nóbrega, Joaquim A

    2004-11-15

    In the present work, thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was employed for Cu and Zn determination in bovine milk and fruit juice samples without any pretreatment. TS-FF-AAS system was optimized and a sample volume of 300mul was injected into the carrier stream (0.014moll(-1) HNO(3) at a flow rate of 0.4mlmin(-1)), and it was introduced into a hot Ni tube. The detection limits obtained for Cu and Zn in aqueous solution were 2.2 and 0.91mugl(-1), respectively, and 3.2mugl(-1) for Cu in a medium containing water-soluble tertiary amines. The relative standard deviations varied from 2.7 to 4.2% (n=12). Sample preparation was carried out by simple dilution in water or in water-soluble tertiary amines medium. Accuracy was checked by performing addition-recovery experiments as well as by using reference materials (whole milk powder, non-fat milk powder, and infant formula). Recoveries varied from 97.7 to 105.3% for Cu and Zn. All results obtained for reference materials were in agreement with certified values at a 95% confidence level.

  9. Determination of vanadium in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry using permanent modifiers.

    PubMed

    Dobrowolski, Ryszard; Adamczyk, Agnieszka; Otto, Magdalena

    2013-09-15

    A new analytical procedure for vanadium (V) determination in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry (slurry sampling GFAAS) using the mixed permanent modifiers is described. Moreover, the comparison of action of the modifiers based on the iridium (Ir) and carbide-forming elements: tungsten (W) and niobium (Nb) deposited on the graphite tubes is studied, especially in terms of their analytical utility and determination sensitivity. The mechanism of their action was investigated using an X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray detector (EDX). Finally, the mixture of 0.3 μg of Ir and 0.04 μg of Nb was used for the graphite tube permanent modification. The analytical procedure was optimized on the basis of the data from pyrolysis and atomization temperature curves studies. The results obtained for the four certified reference materials (marine sediments: PACS-1 and MESS-1, lake sediment: SL-1, soil: San Joaquin Soil SRM 2709), using the slurry sampling GFAAS and the standard calibration method, were in good agreement with the certified values. The detection and quantification limits and characteristic mass calculated for the proposed procedure were 0.04 µg/g, 0.16 µg/g and 11.9 pg, respectively. The precision (RSD% less than 8%) and the accuracy of vanadium determination in the soil and sediment samples were acceptable.

  10. The determination of wear metals in used lubricating oils by flame atomic absorption spectrometry using sulphanilic acid as ashing agent.

    PubMed

    Ekanem, E J; Lori, J A; Thomas, S A

    1997-11-01

    A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of calcium, magnesium, zinc, iron, chromium and nickel by flame atomic absorption spectrometry. Sulphanilic acid was added to oil samples and the mixture coked and the coke ashed at 550 degrees C. The solutions of the ash were analysed by flame AAS for the metals. The release of calcium, zinc, iron and chromium was improved by the addition of sulphanilic acid to samples. The relative standard deviations of metal concentration results in the initial oil samples were 1.5% for Ca (1500 mg l(-1) level), 0.3% for Mg (100 mg l(-1) level), 3.1% for Zn (1500 mg l(-1) level), 0.7% for Fe (500 mg l(-1) level), 0.02% for Cr (50 mg l(-1) level) and 0.002% for Ni (10 mg l(-1) level). The optimum sample size for efficient metal release was 20 g while the optimum sulphanilic acid to oil ratio was 0.05 g per gram of oil for Zn and Cr and 0.10 g for Ca and Fe. Results obtained by this procedure were highly reproducible and comparable with those obtained for the same samples using standard procedures.

  11. Evaluation of ammonia as diluent for serum sample preparation and determination of selenium by graphite furnace atomic absorption spectrometry*1

    NASA Astrophysics Data System (ADS)

    Hernández-Caraballo, Edwin A.; Burguera, Marcela; Burguera, José L.

    2002-12-01

    A method for the determination of total selenium in serum samples by graphite furnace atomic absorption spectrometry was evaluated. The method involved direct introduction of 1:5 diluted serum samples (1% v/v NH 4OH+0.05% w/v Triton X-100 ®) into transversely heated graphite tubes, and the use of 10 μg Pd+3 μg Mg(NO 3) 2 as chemical modifier. Optimization of the modifier mass and the atomization temperature was conducted by simultaneously varying such parameters and evaluating both the integrated absorbance and the peak height/peak area ratio. The latter allowed the selection of compromise conditions rendering good sensitivity and adequate analyte peak profiles. A characteristic mass of 49 pg and a detection limit (3s) of 6 μg 1 -1 Se, corresponding to 30 μg l -1 Se in the serum sample, were obtained. The analyte addition technique was used for calibration. The accuracy was assessed by the determination of total selenium in Seronorm™ Trace Elements Serum Batch 116 (Nycomed Pharma AS). The method was applied for the determination of total selenium in ten serum samples taken from individuals with no known physical affection. The selenium concentration ranged between 79 and 147 μg l -1, with a mean value of 114±22 μg l -1.

  12. Evaluation of oxidant media for the determination of lead in food slurries by hydride generation atomic absorption spectrometry.

    PubMed

    Madrid, Y; Bonilla, M; Cámara, C

    1990-05-01

    Several oxidant media were evaluated for the generation of lead hydride from slurry samples and their application to the determination of lead in vegetables and fish by hydride generation atomic absorption spectrometry. Three oxidant - acid media were compared: hydrogen peroxide - nitric acid, ammonium persulphate - nitric acid and potassium dichromate - lactic acid. The powdered samples were suspended in Triton X-100 and shaken with 10.0 g of blown zirconia spheres until a slurry was formed. The potassium dichromate - lactic acid medium was the most satisfactory for the determination of lead in fish and vegetables, providing the lowest detection limits as a result of its high sensitivity and low blank values. The ammonium persulphate - nitric acid medium gave good accuracy, precision and selectivity for vegetables (1-2 p.p.m. of lead); however, with fish (0.1-1 p.p.m. of lead) it was only a semi-quantitative medium for the determination of lead owing to its lack of sensitivity and selectivity. The hydrogen peroxide - nitric acid medium was unsatisfactory for the generation of lead hydride from slurry samples because of decomposition of hydrogen peroxide by the organic matter in the sample.

  13. Determination of lead and manganese in biological samples and sediment using slurry sampling and flame atomic absorption spectrometry.

    PubMed

    Vieira, Daniel Rodrigues; Castro, Jacira Teixeira; Lemos, Valfredo Azevedo

    2011-01-01

    A procedure was developed for the determination of lead (Pb) and manganese (Mn) using slurry sampling. The two elements were detected using flame atomic absorption spectrometry with a slotted tube atom trap. Slurries were prepared by adding nitric acid solution (0.30%, w/v) to a powdered sample (0.10 g). After homogenization by ultrasonic bath for 15 min, the slurries were introduced directly into the detection equipment. Some conditions of the procedure were evaluated, such as acid concentration, presence of surfactants, and sonication time. Under optimized conditions, the LODs and LOQs achieved were 0.8 and 2.6 microg/g for Pb and 0.5 and 1.6 microg/g for Mn, respectively. The precision obtained varied between 3.1 and 5.8% (Mn), and 2.6 and 5.4% (Pb) for slurries of shrimp and sediment. The analytical curves were established using aqueous standards in nitric acid solutions. The accuracy of the method was assessed through the determination of Pb and Mn in the following certified reference materials: ERM-CE 278 (mussel tissue), CRM 397 (human hair), and SRM 1646a (estuarine sediment). The proposed procedure was successfully applied to the determination of Pb and Mn in six samples of shrimp powder, seasoning, and river sediment. The levels of Mn detected varied from 2.2 to 71.3 microg/g; Pb was detected in only one sediment sample (4.3 microg/g).

  14. [Trace Analysis of Lead in Copper Gluconate by Atomic Absorption Spectrometry after Separation by Co-Precipitation with Bismuth].

    PubMed

    Ito, Michio; Ishiguro, Satoshi; Takahashi, Fumihito; Nomura, Takakazu; Sugimoto, Toshiaki; Nishimura, Tsutomu

    2015-01-01

    In order to determine trace amounts of lead in copper gluconate by atomic absorption spectrometry (AAS), the authors investigated a separation and pre-concentration procedure using a co-precipitation technique with bismuth. After ashing 2.0 g of the sample by means of a dry process, the ash was dissolved in (1→100) nitric acid and 75 μg of bismuth was added. Lead was co-precipitated by using an ammonium solution controlled to pH 9.5-10.5. The precipitate was left at room temperature for over 15 minutes to age, and then washed with a (3→100) ammonium solution three times. The precipitate was dissolved in (1→100) nitric acid and then analyzed by AAS. The quantification limit of this method was 0.5 mg/kg, and the trueness, repeatability and intermediate precision were 99.6%, 4.2% and 4.2% at the spiked concentration of 0.5 mg/kg, and 94.4%, 2.8% and 4.0% at the spiked concentration of 5.0 mg/kg, respectively. Thus, the present method for trace analysis of lead in copper gluconate was validated.

  15. Preconcentration of lead using solidification of floating organic drop and its determination by electrothermal atomic absorption spectrometry

    PubMed Central

    Chamsaz, Mahmoud; Akhoundzadeh, Jeiran; Arbab-zavar, Mohammad Hossein

    2012-01-01

    A simple microextraction method based on solidification of a floating organic drop (SFOD) was developed for preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Ammonium pyrolidinedithiocarbamate (APDC) was used as complexing agent, and the formed complex was extracted into a 20 μL of 1-undecanol. The extracted complex was diluted with ethanol and injected into a graphite furnace. An orthogonal array design (OAD) with OA16 (45) matrix was employed to study the effects of different parameters such as pH, APDC concentration, stirring rate, sample solution temperature and the exposure time on the extraction efficiency. Under the optimized experimental conditions the limit of detection (based on 3 s) and the enhancement factor were 0.058 μg L−1 and 113, respectively. The relative standard deviation (RSD) for 8 replicate determinations of 1 μg L−1 of Pb was 8.8%. The developed method was validated by the analysis of certified reference materials and was successfully applied to the determination of lead in water and infant formula base powder samples. PMID:25685441

  16. Determination of tin and titanium in soils, sediments and sludges using electrothermal atomic absorption spectrometry with slurry sample introduction.

    PubMed

    López-García, Ignacio; Arnau-Jerez, Isabel; Campillo, Natalia; Hernández-Córdoba, Manuel

    2004-02-06

    Fast-heating programmes for determining titanium and tin in soils, sediments and sludges using electrothermal atomic absorption spectrometry (ETAAS) with slurry sampling are developed. For titanium determination, suspensions are prepared by weighing 5-40mg of sample and adding 25ml of a solution containing 50% (v/v) concentrated hydrofluoric acid. For tin determination, suspensions are prepared by weighing up to 300mg of sample and then adding 1ml of a solution containing 25% (v/v) concentrated hydrofluoric acid. Palladium (30mug) and ammonium dihydrogen phosphate (7% w/v) are used as matrix modifiers for titanium and tin, respectively. Prior mild heating in a microwave oven is recommended for titanium determination. Calibration is carried out using aqueous standards. The tin and titanium contents of a number of samples obtained by using the slurry approach agree with those obtained by means of a procedure based on the total dissolution of the samples using microwave oven digestion. The reliability of the procedures is also confirmed by analysing several certified reference materials.

  17. Fast determination of lead in lake sediment samples using electrothermal atomic absorption spectrometry with slurry samples introduction.

    PubMed

    Barałkiewicz, Danuta

    2002-01-04

    Lead concentration in lake sediment samples has been determined by means of ultrasonic slurry sampling electrothermal atomic absorption spectrometry USSS-ETAAS. The soil samples were suspended (0.025-0.15% w/v slurry) in four different liquid media containing 0.5% (v/v) nitric acid, 5% (v/v) nitric acid, 0.5% nitric acid+Triton X-100 and 5% nitric acid+Triton X-100. The effects of the instrumental operating conditions and slurry preparation on the signal were examined. Palladium and magnesium were used as modifiers to improve the signal quality. The procedure was validated by analysis of the certified reference lake sediment material LKSD-1, LKSD-2, LKSD-3 and LKSD-4. All analytical recoveries for lead in slurried lake sediment samples were satisfactory and varied from 95 to 104%. Relative standard deviation (R.S.D.) values were 4.8, 4.7, 4.5 and 5.5. The detection limits LODs of lead were 0.52, 0.45, 0.35, and 0.22 mug g(-1) for mass of sample 0.025, 0.050, 0.10 and 0.15 U, respectively.

  18. Determination of nickel in saliva by electrothermal atomic absorption spectrometry using various chemical modifiers with Zeeman-effect background correction.

    PubMed

    Burguera, E; Sanchez de Briceño, A; Rondon, C E; Burguera, J L; Burguera, M; Carrero, P

    1998-07-01

    The profile of nickel signal using electrothermal atomic absorption spectrometry with deuterium and Zeeman-effect background correction is presented. The Zeeman effect system of background correction offered definitive advantages and therefore was used for the determination of nickel in saliva in the presence of various isomorphous metals. The highest nickel absorbance values corresponded at 200, 300, 300, 300, 600, and 200 ng of Tb, Mg, Sm, Lu, Tm, and Pd, respectively. On the other hand, the addition of Eu, Er, and Ho decreased the nickel signal. The presence on each modifier alone does not eliminate the matrix interference. However, the use of 200 ng of Pd in conjuction with 300 ng of Lu has a higher sensitivity, offers an advantage against interference from the background of saliva matrix and produces good recoveries (98 to 102% from unspiked and spiked saliva samples). The limit of detection was 0.11 micrograms/L for a characteristic mass of 16.6 pg of nickel using Pd-Lu as modifier. The within-batch precision varied between 0.8 and 1.5% relative standard deviations. The analysis of thirty samples of whole saliva gave an average of 0.81 +/- 0.30 of micrograms/L of Ni (range from 0.5 to 2.0 micrograms/L of Ni). The agreement between the observed and certified values obtained from a Seronorm Blood Serum Standard Reference Material was good.

  19. Determination of trace nickel in hydrogenated cottonseed oil by electrothermal atomic absorption spectrometry after microwave-assisted digestion.

    PubMed

    Zhang, Gai

    2012-01-01

    Microwave digestion of hydrogenated cottonseed oil prior to trace nickel determination by electrothermal atomic absorption spectrometry (ETAAS) is proposed here for the first time. Currently, the methods outlined in U.S. Pharmacopeia 28 (USP28) or British Pharmacopeia (BP2003) are recommended as the official methods for analyzing nickel in hydrogenated cottonseed oil. With these methods the samples may be pre-treated by a silica or a platinum crucible. However, the samples were easily tarnished during sample pretreatment when using a silica crucible. In contrast, when using a platinum crucible, hydrogenated cottonseed oil acting as a reducing material may react with the platinum and destroy the crucible. The proposed microwave-assisted digestion avoided tarnishing of sample in the process of sample pretreatment and also reduced the cycle of analysis. The programs of microwave digestion and the parameters of ETAAS were optimized. The accuracy of the proposed method was investigated by analyzing real samples. The results were compared with the ones by pressurized-PTFE-bomb acid digestion and ones obtained by the U.S. Pharmacopeia 28 (USP28) method. The new method involves a relatively rapid matrix destruction technique compared with other present methods for the quantification of metals in oil.

  20. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    PubMed Central

    Daşbaşı, Teslima; Kartal, Şenol; Saçmacı, Şerife; Ülgen, Ahmet

    2016-01-01

    A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4− complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n = 13). The precision as relative standard deviation was 3% (n = 11, 0.20 mg L−1) and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water). PMID:26881186

  1. Determination of Low Levels of Lead in Beer Using Solid-Phase Extraction and Detection by Flame Atomic Absorption Spectrometry

    PubMed Central

    Alves, Vanessa N.; Borges, Simone S. O.; Neto, Waldomiro B.; Coelho, Nívia M. M.

    2011-01-01

    In this study, a method for the determination of low concentrations of lead in beer samples using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry (FAAS) was developed. Moringa oleifera seeds were used as a biosorbent material. Chemical and flow variables of the online preconcentration system, such as sample pH, preconcentration flow rate, eluent flow rate, eluent concentration, particle size, and sorbent mass, were studied. The optimum extraction conditions were obtained using a sample pH of 6.0, sample flow rate of 6.0 mL min−1, 63.0 mg of sorbent mass, and 2.0 mol L−1 HNO3 at a flow rate of 2.0 mL min−1 as the eluent. With the optimized conditions, the preconcentration factor, precision, detection limit, consumption index, and sample throughput were estimated as 93, 0.3% (10.0 μg L−1, n = 7), 7.5 μg L−1, 0.11 mL, and 23 samples per hour, respectively. The method developed was successfully applied to beer samples and recovery tests, with recovery ranging from 80% to 100%. PMID:22013389

  2. Cloud point extraction and flame atomic absorption spectrometry determination of lead (II) in environmental and food samples.

    PubMed

    Soylak, Mustafa; Yilmaz, Erkan; Ghaedi, Mehrorang; Montazerozohori, Mortaza; Sheibani, Marjan

    2012-01-01

    A cloud point extraction procedure for the preconcentration of Pb2+ in various samples following complexation with 2,2'-(1E,1'E)-1,1'-(2,2'-azanediylbis(ethane-2,1-diyl)bis(azan-1-yl-1-ylidene)) bis(ethan-1-yl-1-ylidene)diphenol in Triton X-114 after centrifugation is reported. A 0.5 mL portion of methanol acidified with 1.0 M HNO3 was added to the surfactant-rich phase prior to analysis by flame atomic absorption spectrometry. The influence of analytical parameters--including pH, concentrations of ligand, Triton X-114, and HNO3, bath temperature, heating time, and centrifugation rate and time--were optimized, and the effect of the matrix ions on the recovery of Pb2+ was investigated. An LOD of 1.9 ng/mL along with a preconcentration factor of 50 with RSD of 1.0% for Pb2+ were achieved. The proposed procedure was applied to the analysis of various real samples.

  3. Method development for Cd and Hg determination in biodiesel by electrothermal atomic absorption spectrometry with emulsion sample introduction.

    PubMed

    Aranda, Pedro R; Gásquez, José A; Olsina, Roberto A; Martinez, Luis D; Gil, Raúl A

    2012-11-15

    A novel method for analysis of biodiesel by electrothermal atomic absorption spectrometry is described. This analytical strategy involves sample preparation as emulsions for routine and reliable determination of Cd and Hg. Several experimental conditions were investigated, including emulsion stability and composition, furnace temperature program and matrix modification. Different calibration strategies were also evaluated, being the analyte addition method preferred both for Cd and Hg. The accuracy was verified through comparison with an acid digestion in a microwave closed system. The injection repeatability was evaluated as the average relative standard deviation (R.S.D %) for five successive firings and was better than 4.4% for Cd and 5.4% Hg respectively. The detection limits, evaluated by the 3σ concept of calculation (n=10), were of 10.2 μg kg(-1) (0.9 μg L(-1)) for Hg and 0.3 μg kg(-1) (0.04 μg L(-1)) for Cd. This method was successfully applied to the determination of Cd and Hg in biodiesel samples obtained from local vendors.

  4. Direct determination of silicon in powdered aluminium oxide by use of slurry sampling with in situ fusion graphite-furnace atomic-absorption spectrometry.

    PubMed

    Minami, H; Yoshida, T; Okutsu, K; Zhang, Q; Inoue, S; Atsuya, I

    2001-08-01

    A direct method for determination of silicon in powdered high-purity aluminium oxide samples, by slurry sampling with in situ fusion graphite-furnace atomic-absorption spectrometry (GF-AAS), has been established. A slurry sample was prepared by 10-min ultrasonication of a powdered sample in an aqueous solution containing both sodium carbonate and boric acid as a mixed flux. An appropriate portion of the slurry was introduced into a pyrolytic graphite furnace equipped with a platform. Silicon compounds to be determined and aluminium oxide were fused by the in situ fusion process with the flux in the furnace under optimized heating conditions, and the silicon absorbance was then measured directly. The calibration curve was prepared by use of a silicon standard solution containing the same concentration of the flux as the slurry sample. The accuracy of the proposed method was confirmed by analysis of certified reference materials. The proposed method gave statistically accurate values at the 95% confidence level. The detection limit was 3.3 microg g(-1) in solid samples, when 300 mg/20 mL slurry was prepared and a 10 microL portion of the slurry was measured. The precision of the determination (RSD for more than four separate determinations) was 14% and 2%, respectively, for levels of 10 and 100 microg g(-1) silicon in aluminium oxide.

  5. Automatic kinetic bioaccessibility assay of lead in soil environments using flow-through microdialysis as a front end to electrothermal atomic absorption spectrometry.

    PubMed

    Cocovi-Solberg, David J; Rosende, Maria; Miró, Manuel

    2014-06-03

    In-line microdialysis is in this work hyphenated to electrothermal atomic absorption spectrometry via a dedicated flow-based interface for monitoring the batchwise leaching test endorsed by the Standards, Measurements and Testing Program (SM&T) of the European Commission. The bioaccessible pool of lead in soils is measured using 0.43 mol/L AcOH as extractant. The proposed method allows to gain knowledge of leaching kinetics at real-time, simplify the overall procedure by accurate detection of steady-state conditions and overcome sample filtration or centrifugation. Soil leachates were automatically sampled at specified timeframes (e.g, every 20 or 80 min), processed in an external container (where dilution can be applied at will) and further injected into the atomizer. The method was experimentally validated by comparison of in situ microdialysis sampling results with in-line microfiltration in two soils of varying physicochemical properties. A mathematical framework was used for discrimination of different metal fractions (that is, readily mobilizable against slowly mobilizable lead) and also for estimating the total extractable lead under actual steady-state conditions. We have demonstrated that bioaccessibility tests lasting 16 h as endorsed by SM&T might not suffice for ascertainment of maximum (steady-state) bioaccessibility of lead in terrestrial environments as demanded in risk assessment programs.

  6. Measurement of initial absorption of fused silica at 193nm using laser induced deflection technique (LID)

    NASA Astrophysics Data System (ADS)

    Schönfeld, Dörte; Klett, Ursula; Mühlig, Christian; Thomas, Stephan

    2008-01-01

    The ongoing development in microlithography towards further miniaturization of structures creates a strong demand for lens material with nearly ideal optical properties. Beside the highly demanding requirements on homogeneity and stress induced birefringence (SIB), low absorption is a key factor. Even a small absorption is associated with a temperature increase and results in thermally induced local variations of refractive index and SIB. This could affect the achievable resolution of the lithographic process. The total absorption of the material is composed of initial absorption and of absorption induced during irradiation. Thus, the optimization of both improves the lifetime of the material. In principal, it is possible to measure transmission and scattering with a suitable spectrometer assembly and calculate absorption from them. However, owing to the influence of sample surfaces and errors of measurement, these methods usually do not provide satisfactory results for highly light-transmissive fused silica. Therefore, it is most desirable to find a technique that is capable of directly measuring absorption coefficients in the range of (1...10)•10 -4 cm -1 (base 10) directly. We report our first results for fused silica achieved with the LID technique. Besides a fused silica grade designed for 193 nm applications, grades with higher absorption at 193 nm were measured to test the LID technique. A special focus was set on the possibility of measuring initial absorption without the influence of degradation effects.

  7. Simultaneous determination of iron and nickel in fluoropolymers by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

    Soares, Bruno M; Santos, Rafael F; Bolzan, Rodrigo C; Muller, Edson I; Primel, Ednei G; Duarte, Fabio A

    2016-11-01

    This paper reports the development of a method of simultaneous determination of iron and nickel in fluoropolymers by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with direct solid sampling. In order to carry out simultaneous measurements, both the main resonance line of nickel (232.003nm) and the adjacent secondary line of iron (232.036nm) were monitored in the same spectral window. The proposed method was optimized with a perfluoroalkoxy (PFA) sample and was applied to the determination of iron and nickel in fluorinated ethylene propylene (FEP) and modified polytetrafluoroethylene (PTFE-TFM) samples. Pyrolysis and atomization temperatures, as well as the use of Pd and H2 (during pyrolysis) as chemical modifiers, were carefully investigated. Compromise temperatures for pyrolysis and atomization of both analytes were achieved at 800 and 2300°C, respectively, using only 0.5Lmin(-1) H2 as chemical modifier during pyrolysis. Calibration curves were performed with aqueous standards by using a single solution which contained both analytes. Limits of detection were 221 and 9.6ngg(-1) for iron and nickel, respectively. Analyte concentrations in all samples ranged from 3.53 to 12.4µgg(-1) for iron and from 37 to 78ngg(-1) for nickel, with relative standard deviation less than 19%. Accuracy was evaluated by comparing these results with those obtained by inductively coupled plasma mass spectrometry after sample digestion by microwave-induced combustion and no significant statistical difference was observed.

  8. Measurement of the absorption coefficient using the sound-intensity technique

    NASA Technical Reports Server (NTRS)

    Atwal, M.; Bernhard, R.

    1984-01-01

    The possibility of using the sound intensity technique to measure the absorption coefficient of a material is investigated. This technique measures the absorption coefficient by measuring the intensity incident on the sample and the net intensity reflected by the sample. Results obtained by this technique are compared with the standard techniques of measuring the change in the reverberation time and the standing wave ratio in a tube, thereby, calculating the random incident and the normal incident adsorption coefficient.

  9. Feasibility of using solid sampling graphite furnace atomic absorption spectrometry for speciation analysis of volatile and non-volatile compounds of nickel and vanadium in crude oil.

    PubMed

    Silva, Márcia M; Damin, Isabel C F; Vale, Maria Goreti R; Welz, Bernhard

    2007-03-30

    A method for the direct determination of volatile and non-volatile nickel and vanadium compounds in crude oil without previous treatment using direct solid sampling graphite furnace atomic absorption spectrometry is proposed. The crude oil samples were weighed directly onto solid sampling platforms using a microbalance and introduced into a transversely heated solid sampling graphite tube. In previous work of our group losses of volatile nickel and vanadium compounds have been detected, whereas other nickel and vanadium compounds were thermally stable up to 1300 and 1600 degrees C, respectively. In order to avoid this problem different chemical modifiers (conventional and permanent) have been investigated. With 400microg of iridium as permanent modifier, the signal started to drop already after two atomization cycles, possibly because of an interaction of nickel (which is a catalyst poison) with iridium. Twenty micrograms of palladium applied in each determination was found to be optimum for both elements. The palladium was deposited on the platform and submitted to a drying step at 150 degrees C for 75s. After that the sample was added onto the platform and submitted to the furnace program. The influence of sample mass on the linearity of the response and on potential measurement errors was also investigated using four samples with different nickel content. For the sample with the lowest nickel concentration the relationship between mass and integrated absorbance was found to be non-linear when a high sample mass was introduced. It was suspected that the modifier had not covered the entire platform surface, which resulted in analyte losses. This problem could be avoided by using 40microL of 0.5g L(-1) Pd with 0.05% Triton X-100. Calibration curves were established with and without modifier, with aqueous standards, oil-in-water emulsions and the certified reference material NIST SRM 1634c (trace metals in residual fuel oil). The sensitivity for aqueous standards

  10. A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry for analysis of samples with high NaCl contents

    NASA Astrophysics Data System (ADS)

    Čánský, Zdeněk; Rychlovský, Petr; Petrová, Zuzana; Matousek, J. P.

    2007-03-01

    A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry has been developed for determination of lead and cadmium in samples with high salt contents. To separate the analyte from the sample matrix, the analyte was in-situ quantitatively electrodeposited on a platinum sampling capillary serving as the cathode (sample volume, 20 μL). The spent electrolyte containing the sample matrix was then withdrawn, the capillary with the analyte deposited was washed with deionized water and the analyte was stripped into a chemically simple electrolyte (5 g/L NH 4H 2PO 4) by reversing the polarity of the electrodeposition circuit. Electrothermal atomization using a suitable optimized temperature program followed. A fully automated manifold was designed for this coupled technique and the appropriate control software was developed. The operating conditions for determination of Pb and Cd in samples with high contents of inorganic salts were optimized, the determination was characterized by principal analytical parameters and its applicability was verified on analyses of urine reference samples. The absolute limits of detection for lead and cadmium (3 σ criterion) in a sample containing 30 g/L NaCl were 8.5 pg and 2.3 pg, respectively (peak absorbance) and the RSD values amounted to 1.6% and 1.9% for lead (at the 40 ng mL - 1 level) and cadmium (at the 4.0 ng mL - 1 level), respectively. These values (and also the measuring sensitivity) are superior to the results attained in conventional electrothermal atomic absorption spectrometric determination of Pb and Cd in pure solutions (5 g/L NH 4H 2PO 4). The sensitivity of the Pb and Cd determination is not affected by the NaCl concentration up to a value of 100 g/L, demonstrating an efficient matrix removal during the electrodeposition step.

  11. Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry.

    PubMed

    Gómez-Nieto, Beatriz; Gismera, Ma Jesús; Sevilla, Ma Teresa; Procopio, Jesús R

    2015-01-07

    The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample.

  12. Determination of chlorine via the CaCl molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis.

    PubMed

    Guarda, Ananda; Aramendía, Maite; Andrés, Irene; García-Ruiz, Esperanza; do Nascimento, Paulo Cícero; Resano, Martín

    2017-01-01

    This work investigates the possibilities of high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of Cl in solid samples via the CaCl molecule and measurement of its molecular absorption. The method proposed is based on addition of 400µg Ca as molecule-forming reagent and of 20µgPd as chemical modifier, which helps to stabilize the analyte and enhances sensitivity. The molecular spectrum for CaCl offers different lines with different limits of detection and linear ranges, which permitted to analyze solid samples with different Cl contents. The lowest limit of detection (0.75ng Cl, corresponding to 0.75µgg(-1) for a typical sample mass of 1mg) could be achieved by combination of three of the most sensitive lines in the vicinity of 620.862nm, while the amplest linear range (up to 860ng Cl) was achieved by selection of the less sensitive line at 377.501nm. The method developed enabled the direct determination of Cl in solid samples using simple external calibration with aqueous standards. Good precision (5-9% RSD) and accuracy was attained in a series of certified samples of very different nature (i.e. coal, iron oxide, polyethylene, human hair, pine needles, rice flour and milk) and with very different Cl contents, ranging from about 50µgg(-1) to 1% (w/w) Cl. The method appears as particularly useful for Cl determination in samples with elevated Ca contents, for which biased results with other diatomic molecules, such as AlCl or SrCl, may be obtained.

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

    NASA Astrophysics Data System (ADS)

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

    2009-06-01

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

  14. Pseudopotential calculations and photothermal lensing measurements of two-photon absorption in solids

    SciTech Connect

    White, W.T. III

    1985-11-04

    We have studied two-photon absorption in solids theoretically and experimentally. We have shown that it is possible to use accurate band structure techniques to compute two-photon absorption spectra within 15% of measured values in a wide band-gap material, ZnS. The empirical pseudopotential technique that we used is significantly more accurate than previous models of two-photon absorption in zinc blende materials, including present tunneling theories (which are essentially parabolic-band results in disguise) and the nonparabolic-band formalism of Pidgeon et al. and Weiler. The agreement between our predictions and previous measurements allowed us to use ZnS as a reference material in order to validate a technique for measuring two-photon absorption that was previously untried in solids, pulsed dual-beam thermal lensing. With the validated technique, we examined nonlinear absorption in one other crystal (rutile) and in several glasses, including silicates, borosilicates, and one phosphate glass. Initially, we believed that the absorption edges of all the materials were comparable; however, subsequent evidence suggested that the effective band-gap energies of the glasses were above the energy of two photons in our measurement. Therefore, we attribute the nonlinear absorption that we observed in glasses to impurities or defects. The measured nonlinear absorption coefficients were of the order of a few cm/TW in the glasses and of the order of 10 cm/GW in the crystals, four orders of magnitude higher than in glasses. 292 refs.

  15. Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination.

    PubMed

    Molaakbari, Elaheh; Mostafavi, Ali; Afzali, Daryoush

    2011-01-30

    In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 μL ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL(-1), the detection limit was 0.37 ng mL(-1) (3S(b)/m, n = 7) and the relative standard deviation was ±1.63% (n = 7, C = 200 ng mL(-1)). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

  16. Study of the roles of chemical modifiers in determining boron using graphite furnace atomic absorption spectrometry and optimization of the temperature profile during atomization.

    PubMed

    Yamamoto, Yuhei; Shirasaki, Toshihiro; Yonetani, Akira; Imai, Shoji

    2015-01-01

    The measurement conditions for determining boron using graphite furnace-atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L(-1) when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS.

  17. Solid phase extraction of mercury on sulfur loaded with N-(2-chloro benzoyl)-N'-phenylthiourea as a new adsorbent and determination by cold vapor atomic absorption spectrometry.

    PubMed

    Pourreza, N; Parham, H; Kiasat, A R; Ghanemi, K; Abdollahi, N

    2009-06-15

    This paper reports sulfur powder loaded with N-(2-chloro benzoyl)-N'-phenylthiourea as a new solid phase extractor for determination of ultra trace amounts of mercury. The mercury ions were retained on a mini-column filled with the solid phase at a flow rate of 16 mL min(-1). The retained Hg(II) ions were eluted with 3 mol L(-1) solution of HCl and measured by cold vapor atomic absorption spectrometry (CV-AAS). The mercury vapors were generated by a homemade Reaction Cell-Gas Liquid Separator (RC-GLS). The effect of different variables such as pH, sample flow rate, amounts of ligand loaded on sulfur and SnCl2 concentration was investigated. Calibration curve was linear in the range of 0.02-1.20 microg L(-1) with r=0.9991 (n=8). The limit of detection (LOD) based on three times the standard deviation of the blank was 0.012 and 0.003 microg L(-1) when 250 and 1000 mL sample volumes were used, respectively. The relative standard deviation (R.S.D.) for determination of 0.04 and 1.00 microg L(-1) of Hg(II) was 3.9 and 1.2% (n=8), respectively. The method was successfully applied to determine Hg(II) in water and marine samples.

  18. Feasibility of using in situ fusion for the determination of Co, Cr and Mn in Portland cement by direct solid sampling graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Intima, Danielle Polidorio; de Oliveira, Elisabeth; Oliveira, Pedro Vitoriano

    2009-06-01

    In situ fusion on the boat-type graphite platform has been used as a sample pretreatment for the direct determination of Co, Cr and Mn in Portland cement by solid sampling graphite furnace atomic absorption spectrometry (SS-GF AAS). The 3-field Zeeman technique was adopted for background correction to decrease the sensitivity during measurements. This strategy allowed working with up to 200 µg of sample. The in situ fusion was accomplished using 10 µL of a flux mixture 4.0% m/v Na 2CO 3 + 4.0% m/v ZnO + 0.1% m/v Triton® X-100 added over the cement sample and heated at 800 °C for 20 s. The resulting mould was completely dissolved with 10 µL of 0.1% m/v HNO 3. Limits of detection were 0.11 µg g - 1 for Co, 1.1 µg g - 1 for Cr and 1.9 µg g - 1 for Mn. The accuracy of the proposed method has been evaluated by the analysis of certified reference materials. The values found presented no statistically significant differences compared to the certified values (Student's t-test, p < 0.05). In general, the relative standard deviation was lower than 12% ( n = 5).

  19. Determination of sulfur in crude oil using high-resolution continuum source molecular absorption spectrometry of the SnS molecule in a graphite furnace.

    PubMed

    Cadorim, Heloisa R; Pereira, Éderson R; Carasek, Eduardo; Welz, Bernhard; de Andrade, Jailson B

    2016-01-01

    An analytical method for the determination of sulfur, as the tin mono-sulfide (SnS) molecule, in crude oil using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The molecular absorbance of the SnS has been measured using the wavelength at 271.624 nm and the crude oil samples were prepared as micro-emulsions due to their high viscosity. Several chemical modifiers (Ir, Pd, Ru, Zr) were tested and palladium was chosen, because it exhibited the best performance. The heating program was optimized by comparing the pyrolysis and vaporization curves obtained for an aqueous sulfur standard and a micro-emulsion of a crude oil certified reference material (CRM). The optimum pyrolysis and vaporization temperatures were found to be 600 and 2000°C, respectively. The limit of detection and the characteristic mass using micro-emulsion analysis of crude oil samples were 5.8 and 13.3 ng S. Accuracy and precision of the method has been evaluated using two crude oil CRM (NIST 2721 and NIST 2722), showing good agreement with the informed or certified values.

  20. Sensitive determination of bismuth by flame atomic absorption spectrometry using atom trapping in a slotted quartz tube and revolatilization with organic solvent pulse

    NASA Astrophysics Data System (ADS)

    Kılınç, Ersin; Bakırdere, Sezgin; Aydın, Fırat; Ataman, O. Yavuz

    2012-07-01

    Sensitivity of flame atomic absorption spectrometry (FAAS) for Bi determination was improved by slotted quartz tube (SQT) that was used also for atom trapping (AT). The trapped analyte was released by aspirating a small volume of organic solvent after a reasonable analyte collection time. Sensitivity was improved by 2.9 times by SQT-FAAS and 256 times by SQT-AT-FAAS with respect to FAAS. Optimum trapping period was found to be 6.0 min (36.0 mL of solution). Limit of detection (LOD) for SQT-AT-FAAS was found to be 1.6 ng mL- 1. %RSD was calculated as 4.0% for five replicate measurements of 7.5 ng mL- 1 Bi by SQT-AT-FAAS. Accuracy of the method developed was checked by analyzing a standard reference material of simulated fresh water (NIST 1643e) and result found was in good agreement with the certified one. The method can be applied in any laboratory equipped with a flame AA spectrometer. The consumption of time and sample volume is fairly low and application is simple and easy.

  1. Determination of macro and trace elements in multivitamin dietary supplements by high-resolution continuum source graphite furnace atomic absorption spectrometry with slurry sampling.

    PubMed

    Krawczyk, Magdalena

    2014-01-01

    In this research, three different commercially available multivitamin dietary supplements were analyzed by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) with slurry sampling. The concentrations of Cr, Cu, Fe, Mn, and Se were determined and compared to the amounts stated by producers. The safety of multivitamin dietary supplements depends on various factors including the manufacturing process and the purity and origins of the raw ingredients. For this reason, this research determined concentrations of several toxic elements (As, Cd, and Pb). Microwave-assisted high pressure Teflon bomb digestion was used to determine total amounts of elements in samples. Samples were prepared as slurries at a concentration of 0.1% (m/v) for macro elements (Cr, Cu, Fe, Mn, and Se) and at a concentration of % (m/v) for trace elements (As, Cd, and Pb) in acidic media (3M HNO3). The influence of acid concentration, Triton X-100 addition, sonication time, and sonication power on absorbance was investigated. The accuracy of this method was validated by analyses of NRCC LUTS-1 (Lobster hepatopancreas), NRCC DORM-1 (Dogfish Muscle), NRCC DOLT-2 (Dogfish Liver), NBS SRM 1570 (Spinach Leaves) and NBS SRM 1573 (Tomato Leaves) certified reference materials. The measured elements contents in these reference materials (except NRCC DOLT-2) were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level.

  2. [Direct determination of lead and cadmium in soil by slurry-sampling graphite furnace atomic absorption spectrometry using matrix modification technique].

    PubMed

    Sun, Han-Wen; Wen, Xiao-Hua; Liang, Shu-Xuan

    2006-05-01

    A method for the direct determination of lead and cadmium in soil by slurry-sampling graphite furnace-atomic absorption spectrometry using NH4 H2 PO4 as matrix modifier was developed. The effects of slurry stability, particle size of sample, matrix modifiers, ashing temperature, atomization temperature and common coexistent components on the signal intensities of lead and cadmium were investigated. The apparent activation energies of lead and cadmium were measured based on the linear relationship between the logarithm value of atomization peak time and atomization temperature. The mechanism of matrix modification was discussed. Under optimized conditions, the detection limit was 9.05 x 10(-10) g x mL(-1) for Pb and 1.76 x 10(-11) g x mL(-1) for Cd. The recoveries were in the range of 91%-97% for Pb and 93%-109% for Cd. The relative standard deviations were in the range of 4.2%-7.8%.

  3. Validation of a digestion system using a digester block/cold finger system for the determination of lead in vegetable foods by electrothermal atomic absorption spectrometry.

    PubMed

    De Jesus, Robson M; Junior, Mario M S; Matos, Geraldo D; Dos Santos, Ana M P; Ferreira, Sérgio L C

    2011-01-01

    This paper presents the validation of a system for sample digestion using a digester block/cold finger to determine the lead content in vegetables by electrothermal atomic absorption spectrometry (ETAAS). After mineralization, lead contents were determined by ETAAS using a calibration curve based on aqueous standards prepared in 2.60 M nitric acid solutions containing 5 microg ammonium phosphate as chemical modifier. A pyrolysis temperature of 900 degrees C and atomization temperature of 2000 degrees C were used. This method allowed the determination of lead with a characteristic mass of 35 pg; LOD and LOQ of 0.6 and 2 nglg, respectively, were found. The precision was investigated in terms of reproducibility and repeatability. Reproducibility was estimated by analysis of nine different portions of a certified reference material (CRM) of spinach leaves, and the repeatability was determined through the analysis of nine aliquots of the same solution. The reproducibility and repeatability were found to be 4.27 and 2.94% RSD, respectively. The accuracy was confirmed by analysis of whole meal flour, spinach leaves, and orchard leaves CRMs, all furnished by the National Institute of Standards and Technology. Lead contents were measured using the newly developed technique in 11 different potato samples. The lead contents ranged from 12.80 to 69.27 ng/g, with an average value of 28.59 ng/g. These values were in agreement with data reported in the literature.

  4. Study of ammonium molybdate to minimize the phosphate interference in the selenium determination by electrothermal atomic absorption spectrometry with deuterium background correction

    NASA Astrophysics Data System (ADS)

    Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Adela

    2002-02-01

    The use of ammonium molybdate to minimize the phosphate interference when measuring selenium by electrothermal atomic absorption spectrometry (ETAAS) with deuterium background correction was evaluated. Ammonium molybdate did not produce a selenium thermal stabilization; however, the presence of ammonium molybdate decreased the phosphate interference. The study was carried out with mussel acid digests and mussel slurries. Pd-Mg(NO 3) 2 was used as a chemical modifier at optimum concentrations of 300 and 250 mg l -1, respectively, yielding optimum pyrolysis and atomization temperatures of 1200 and 2100 °C, respectively. A yellow solid (ammonium molybdophosphate) was obtained when adding ammonium molybdate to mussel acid digest solutions. This precipitate can be removed after centrifugation prior to ETAAS determination. Additionally, studies on the sampling of the solid ammonium molybdophosphate (AMP) together with the liquid phase, as a slurry, were also developed. The volatilization of the solid AMP was not reached at temperatures lower than 2500 °C. By this way, phosphate, as AMP, is not present in the vapor phase at the atomization temperature (2100 °C), yielding a reduction of the spectral interference by phosphate. The proposed method was validated analyzing three reference materials of marine origin (DORM-1, DOLT-1 and TORT-1). Good agreement with the certified selenium contents was reached for all cases.

  5. Green Preconcentration of Trace Amounts of Copper from Water and Food Samples onto Novel Organo-Nanoclay Prior to Flame Atomic Absorption Spectrometry.

    PubMed

    Beyki, Mostafa Hossein; Shemirani, Farzaneh; Khani, Rouhollah

    2014-01-01

    In this work, the nanoclay was intercalated with acyclovir (9-[(2-hydroxyethoxy) methyl] guanine), the toxicity of which to mammalian cells is very low. We used no organic solvents for preparation of modified clay and desorption of Cu ions from the sorbent. Batch and column methods were used, and sorption of Cu was quantitative (>98%) in the pH range of 7.5 to 10.0. Quantitative desorption occurred with 5.0 mL of 3.0 M HCl, and the amount of Cu(II) was measured by using flame atomic absorption spectrometry. In the initial solution the linear dynamic range and the LOD were 3.0-1000.0 and 0.58 μg/L, respectively. With 500.0 mL of sample, an enrichment factor of 100 was obtained. The RSD was 2.0% (n = 8, concentration = 0.5 mg/L), and the maximum capacity of the sorbent was 45.0 mg/g. The influence of experimental parameters including sample pH, ionic strength, type and volume of the eluent, and interference of some ions on the recoveries of Cu was investigated. The proposed method using a new and easier prepared solid sorbent was applied to the determination of Cu in different real samples with satisfactory results.

  6. Investigation of chemical modifiers for sulfur determination in diesel fuel samples by high-resolution continuum source graphite furnace molecular absorption spectrometry using direct analysis

    NASA Astrophysics Data System (ADS)

    Huber, Charles S.; Vale, Maria Goreti R.; Welz, Bernhard; Andrade, Jailson B.; Dessuy, Morgana B.

    2015-06-01

    High-resolution continuum source graphite furnace molecular absorption spectrometry has been applied for sulfur determination in diesel fuel. The sharp rotational lines of the carbon monosulfide molecule (formed during the vaporization step) were used to measure the absorbance. The analytical line at 258.056 nm was monitored using the sum of three pixels. Different chemical modifiers were investigated and the mixture of palladium and magnesium was used as chemical modifier in combination with iridium as permanent modifier. L-Cysteine was chosen as sulfur standard and the calibration was done against aqueous standard solutions. The proposed method was applied for the analyses of four diesel samples: two S10 samples and two S500 samples. The trueness of the method was checked with a certified reference material (CRM) of sulfur in diesel fuel (NIST 2724b). Accurate results, for samples and CRM, were achieved after a dilution with propan-1-ol. The following figures of merit were obtained: characteristic mass of 17 ± 3 ng, limit of detection and limit of quantification of 1.4 mg kg- 1 and 4.7 mg kg- 1, respectively.

  7. Oscillator strength measurements of atomic absorption lines from stellar spectra

    NASA Astrophysics Data System (ADS)

    Lobel, Alex

    2011-05-01

    Herein we develop a new method to determine oscillator strength values of atomic absorption lines with state-of-the-art detailed spectral synthesis calculations of the optical spectrum of the Sun and of standard spectral reference stars. We update the log(gf) values of 911 neutral lines observed in the KPNO-FTS flux spectrum of the Sun and high-resolution echelle spectra (R = 80 000) of Procyon (F5 IV-V) and Eps Eri (K2 V) observed with large signal-to-noise (S/N) ratios of 2000 using the new Mercator-Hermes spectrograph at La Palma Observatory (Spain). We find for 483 Fe I, 85 Ni I, and 51 Si I absorption lines in the sample a systematic overestimation of the literature log(gf) values with central line depths below 15%. We employ a curve-of-growth analysis technique to test the accuracy of the new oscillator strength values and compare calculated equivalent line widths to the Moore, Minnaert, and Houtgast atlas of the Sun. The online SpectroWeb database at http://spectra.freeshell.org interactively displays the observed and synthetic spectra and provides the new log(gf) values together with important atomic line data. The graphical database is under development for stellar reference spectra of every spectral sub-class observed with large spectral resolution and S/N ratios.

  8. Acoustic absorption measurement of human hair and skin within the audible frequency range.

    PubMed

    Katz, B F

    2000-11-01

    Utilizing the two-microphone impedance tube method, the acoustic absorption of human skin and hair is measured in the frequency range 1-6 kHz. Various locations on a number of human subjects are measured to determine if the presence of bone or an air pocket affects the acoustic absorption of human skin. The absorption coefficient of human hair is also measured. Additional techniques are utilized to minimize errors due to sample mounting methods. Techniques are employed to minimize potential errors in sensor and sample locations. The results of these measurements are compared to relevant historical papers on similar investigations. Results for skin measurements compare well with previous work. Measured hair absorption data do not agree with previous work in the area but do coincide with expected trends, which previous works do not.

  9. Photoacoustic technique for simultaneous measurements of thermal effusivity and absorptivity of pigments in liquid solution.

    PubMed

    Balderas-López, J A; Díaz-Reyes, J; Zelaya-Angel, O

    2011-12-01

    A photoacoustic (PA) methodology, in the transmission configuration, for simultaneous measurements of thermal effusivity and molar absorption coefficient (absorptivity) for pigments in liquid solution is introduced. The analytical treatment involves a self-normalization procedure for the PA signal, as a function of the modulation frequency, for a strong absorbing material in the thermally thin regime, when the light travels across the sample under study. Two fitted parameters are obtained from the analysis of the self-normalized PA amplitude and phase, one of them proportional to the sample's optical absorption coefficient and from which, taking it for a series of samples at different concentrations, the pigment's absorptivity in liquid solution can be measured, the other one yields the sample's thermal effusivity. Methylene blue's absorptivity in distilled water was measured with this methodology at 658 nm, finding good agreement with the corresponding one reported in the literature.

  10. Sensitive and absolute absorption measurements in optical materials and coatings by laser-induced deflection technique

    NASA Astrophysics Data System (ADS)

    Mühlig, Christian; Bublitz, Simon

    2012-12-01

    The laser-induced deflection (LID) technique, a photo-thermal deflection setup with transversal pump-probe-beam arrangement, is applied for sensitive and absolute absorption measurements of optical materials and coatings. Different LID concepts for bulk and transparent coating absorption measurements, respectively, are explained, focusing on providing accurate absorption data with only one measurement and one sample. Furthermore, a new sandwich concept is introduced that allows transferring the LID technique to very small sample geometries and to significantly increase the sensitivity for materials with weak photo-thermal responses. For each of the different concepts, a representative application example is given. Particular emphasis is placed on the importance of the calibration procedure for providing absolute absorption data. The validity of an electrical calibration procedure for the LID setup is proven using specially engineered surface absorbing samples. The electrical calibration procedure is then applied to evaluate two other approaches that use either doped samples or highly absorptive reference samples.

  11. Determination of toxic elements in plastics from waste electrical and electronic equipment by slurry sampling electrothermal atomic absorption spectrometry.

    PubMed

    Santos, Mirian C; Nóbrega, Joaquim A; Baccan, Nivaldo; Cadore, Solange

    2010-06-15

    Cadmium, chromium, lead and antimony were determined in slurries prepared using pulverized samples of personal computers and mobile phones dispersed in dimethylformamide medium. Determinations were carried out by electrothermal atomic absorption spectrometry (ETAAS) using a graphite furnace atomic absorption spectrometer. The optimization of the experimental conditions (chemical modifier, pyrolysis time, pyrolysis temperature and atomization temperatures) was accomplished by evaluating pyrolysis and atomization curves. Optimization was also used to determine the temperatures corresponding to the best sensitivities and the lowest background signals. The pyrolysis temperatures were fixed at 600 degrees C (for Cd), 700 degrees C (for Pb), 1100 degrees C (for Sb), and 1200 degrees C (for Cr); atomization temperatures were established as 1400 degrees C (for Cd), 1300 degrees C (for Pb), 1900 degrees C (for Sb), and 2300 degrees C (for Cr), and the chemical modifier (50microg NH(4)H(2)PO(4)+3microg Mg(NO(3))(2) was used for Cd and Pb while 5microg Pd+3microg Mg(NO(3))(2) was used for Sb). The use of a chemical modifier for Cr determination was not necessary. The characteristic masses were 1.9pg for Cd, 32.3pg for Pb, 54.1pg for Sb, and 9.1pg for Cr. Calibration was performed using standard additions in a range of 5-20microgL(-1) for Cd, 5-30microgL(-1) for Cr, 12.5-50microgL(-1) for Pb, and 25-100microgL(-1) for Sb with linear correlation coefficients higher than 0.99. Limits of detection were 0.9, 1.4, 6.8, and 2.9microgL(-1) for Cd, Pb, Sb, and Cr, respectively. The results indicate that recoveries for all metals agreed at a 95% confidence level when a paired t-test was applied and presented good precision. The accuracy of the proposed method was evaluated by addition-recovery experiments, showing results in the 96-112% range, and also by comparison of the results using Student's t-test with another method developed using ETAAS for digested samples. Analyte

  12. Direct measurements of nonlinear absorption and refraction in solutions of phthalocyanines

    NASA Technical Reports Server (NTRS)

    Wei, T. H.; Hagan, D. J.; Sence, M. J.; Van Stryland, E. W.; Perry, J. W.; Coulter, D. R.

    1992-01-01

    Direct measurements are reported of the excited singlet-state absorption cross section and the associated nonlinear refractive cross section using picosecond pulses at 532 nm in solutions of phthalocyanine and naphthalocyanine dyes. By monitoring the transmittance and far-field spatial beam distortion for different pulsewidths in the picosecond regime, it is shown that both the nonlinear absorption and refraction are fluence (energy-per-unit-area) rather than irradiance dependent. Thus, excited-state absorption is the dominant nonlinear absorption process, and the observed nonlinear refraction is also due to real population excitation.

  13. Absorption coefficient measurements of particle-laden filters using laser heating: Validation with nigrosin

    NASA Astrophysics Data System (ADS)

    Presser, Cary

    2012-05-01

    A laser-heating technique, referred as the laser-driven thermal reactor, was used in conjunction with laser transmissivity measurements to determine the absorption coefficient of particle-laden substrates (e.g., quartz-fiber filters). The novelty of this approach is that it analyzes a wide variety of specific samples (not just filtered samples) and overcomes measurement issues (e.g., absorption enhancement) associated with other filter-based particle absorption techniques. The absorption coefficient was determined for nigrosin-laden, quartz-fiber filters and the effect of the filter on the absorption measurements was estimated when compared to the isolated nigrosin results. The isolated nigrosin absorption coefficient compared favorably with Lorenz-Mie calculations for an idealized polydispersion of spherical particles (based on a measured nigronsin/de-ionized water suspension size distribution) dispersed throughout a volume equivalent to that of the nigrosin-laden filter. To validate the approach, the absorption coefficient of a nigrosin/de-ionized water suspension was in good agreement with results obtained from an ultraviolet/visible spectrometer. In addition, the estimated imaginary part of the refractive index from the Lorenz-Mie calculations compared well with literature values and was used to estimate the absorption coefficient of optically opaque packed nigrosin.

  14. Contactless nondestructive measurement of bulk and surface recombination using frequency-modulated free carrier absorption

    NASA Astrophysics Data System (ADS)

    Sanii, F.; Giles, F. P.; Schwartz, R. J.; Gray, J. L.

    1992-03-01

    A measurement procedure is described which allows the contactless measurement of bulk lifetime and surface recombination. The procedure uses the the free-carrier absorption of a long-wavelength laser beam by a modulated free-carrier wave to measure and separate the bulk recombination from the surface recombination. The dependence of the absorption on the modulation frequency is used to accomplish the separation. Limitations of the technique are also discussed.

  15. Determination of silicon and aluminum in silicon carbide nanocrystals by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

    Dravecz, Gabriella; Bencs, László; Beke, Dávid; Gali, Adam

    2016-01-15

    The determination of Al contaminant and the main component Si in silicon carbide (SiC) nanocrystals with the size-distribution of 1-8nm dispersed in an aqueous solution was developed using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS). The vaporization/atomization processes were investigated in a transversally heated graphite atomizer by evaporating solution samples of Al and Si preserved in various media (HCl, HNO3). For Si, the best results were obtained by applying a mixture of 5µg Pd plus 5µg Mg, whereas for Al, 10µg Mg (each as nitrate solution) was dispensed with the samples, but the results obtained without modifier were found to be better. This way a maximum pyrolysis temperature of 1200°C for Si and 1300°C for Al could be used, and the optimum (compromise) atomization temperature was 2400°C for both analytes. The Si and Al contents of different sized SiC nanocrystals, dispersed in aqueous solutions, were determined against aqueous (external) calibration standards. The correlation coefficients (R values) of the calibrations were found to be 0.9963 for Si and 0.9991 for Al. The upper limit of the linear calibration range was 2mg/l Si and 0.25mg/l Al. The limit of detection was 3µg/l for Si and 0.5µg/l for Al. The characteristic mass (m0) was calculated to be 389pg Si and 6.4pg Al. The Si and Al content in the solution samples were found to be in the range of 1.0-1.7mg/l and 0.1-0.25mg/l, respectively.

  16. Speciation of platinum in blood plasma and urine by micelle-mediated extraction and graphite furnace atomic absorption spectrometry.

    PubMed

    Mortada, Wael I; Hassanien, Mohammed M; El-Asmy, Ahmed A

    2013-10-01

    A highly sensitive and selective technique for the speciation of platinum by cloud point extraction prior to determination by graphite furnace atomic absorption spectrometry (GFAAS) was described. The separation of Pt(II) from Pt(IV) was performed in the presence of 4-(p-chlorophenyl)-1-(pyridin-2-yl)thiosemicarbazide (HCPTS) as chelating agent and Triton X-114 as a non-ionic surfactant. The extraction of Pt(II)-HCPTS complex needs temperature higher than the cloud point temperature of Triton X-114 and pH = 7, while Pt(IV) remains in the aqueous phase. The Pt(II) in the surfactant phase was analyzed by GFAAS, and the concentration of Pt(IV) was calculated by subtraction of Pt(II) from total platinum which was directly determined by GFAAS. The effect of pH, concentration of chelating agent, surfactant, and equilibration temperature were investigated. An enrichment factor of 42 was obtained for the preconcentration of Pt(II) with 50 mL solution. Under the optimum experimental conditions, the calibration curve was linear up to 30 μgL(-1) with detection limit of 0.08 μgL(-1) and the relative standard deviation was 1.8%. No considerable interference was observed due to the presence of coexisting anions and cations. The accuracy of the results was verified by analyzing different spiked samples (tap water, blood plasma and urine). The proposed method was applied to the speciation analysis of Pt in blood plasma and urine with satisfactory results.

  17. Determination of some heavy metal levels in soft drinks on the Ghanaian market using atomic absorption spectrometry method.

    PubMed

    Ackah, Michael; Anim, Alfred Kwablah; Zakaria, Nafisatu; Osei, Juliet; Saah-Nyarko, Esther; Gyamfi, Eva Tabuaa; Tulasi, Delali; Enti-Brown, Sheriff; Hanson, John; Bentil, Nash Owusu

    2014-12-01

    Twenty-three soft drink samples (i.e., four pineapple-based fruit drinks, eight citrus-based fruit juices, one soya-based drink, three cola carbonated drinks, one apple-based fruit drink, and six cocktail fruit drinks) were randomly purchased from retail outlets in an urban market in Accra and analyzed for the concentrations of iron, cobalt, cadmium, zinc, lead, and copper using flame atomic absorption spectrometry. The mean concentration of iron and cadmium were 0.723 ± 0.448 mg/L and 0.032 ± 0.012 mg/L, respectively. The mean cobalt concentration was 0.071 ± 0.049 mg/L, while the mean Zn concentration in the samples was 0.060 ± 0.097 mg/L. The mean concentrations of Pb and Cu in the fruit juice samples were 0.178 ± 0.091 mg/L and 0.053 ± 0.063 mg/L respectively. About 78 % of the samples exceeded the United States Environmental Protection Agency (USEPA) maximum contaminant level of 0.3 mg/L prescribed for iron, whereas all the samples exceeded the USEPA maximum contaminant level of 0.005 mg/L prescribed for cadmium. About 91 % of the samples exceeded the EU maximum contaminant level prescribed for lead insoft drinks.

  18. Restricted access carbon nanotubes for direct extraction of cadmium from human serum samples followed by atomic absorption spectrometry analysis.

    PubMed

    Barbosa, Adriano F; Barbosa, Valéria M P; Bettini, Jefferson; Luccas, Pedro O; Figueiredo, Eduardo C

    2015-01-01

    In this paper, we propose a new sorbent that is able to extract metal ions directly from untreated biological fluids, simultaneously excluding all proteins from these samples. The sorbent was obtained through the modification of carbon nanotubes (CNTs) with an external bovine serum albumin (BSA) layer, resulting in restricted access carbon nanotubes (RACNTs). The BSA layer was fixed through the interconnection between the amine groups of the BSA using glutaraldehyde as cross-linker. When a protein sample is percolated through a cartridge containing RACNTs and the sample pH is higher than the isoelectric point of the proteins, both proteins from the sample and the BSA layer are negatively ionized. Thus, an electrostatic repulsion prevents the interaction between the proteins from the sample on the RACNTs surface. At the same time, metal ions are adsorbed in the CNTs (core) after their passage through the chains of proteins. The Cd(2+) ion was selected for a proof-of-principle case to test the suitability of the RACNTs due to its toxicological relevance. RACNTs were able to extract Cd(2+) and exclude almost 100% of the proteins from the human serum samples in an online solid-phase extraction system coupled with thermospray flame furnace atomic absorption spectrometry. The limits of detection and quantification were 0.24 and 0.80 μg L(-1), respectively. The sampling frequency was 8.6h(-1), and the intra- and inter-day precisions at the 0.80, 15.0, and 30.0 μg L(-1) Cd(2+) levels were all lower than 10.1% (RSD). The recoveries obtained for human blood serum samples fortified with Cd(2+) ranged from 85.0% to 112.0%. The method was successfully applied to analyze Cd(2+) directly from six human blood serum samples without any pretreatment, and the observed concentrations ranged from

  19. Determination of calcium, magnesium and zinc in lubricating oils by flame atomic absorption spectrometry using a three-component solution.

    PubMed

    Zmozinski, Ariane V; de Jesus, Alexandre; Vale, Maria G R; Silva, Márcia M

    2010-12-15

    Lubricating oils are used to decrease wear and friction of movable parts of engines and turbines, being in that way essential for the performance and the increase of that equipment lifespan. The presence of some metals shows the addition of specific additives such as detergents, dispersals and antioxidants that improve the performance of these lubricants. In this work, a method for determination of calcium, magnesium and zinc in lubricating oil by flame atomic absorption spectrometry (F AAS) was developed. The samples were diluted with a small quantity of aviation kerosene (AVK), n-propanol and water to form a three-component solution before its introduction in the F AAS. Aqueous inorganic standards diluted in the same way have been used for calibration. To assess the accuracy of the new method, it was compared with ABNT NBR 14066 standard method, which consists in diluting the sample with AVK and in quantification by F AAS. Two other validating methods have also been used: the acid digestion and the certified reference material NIST (SRM 1084a). The proposed method provides the following advantages in relation to the standard method: significant reduction of the use of AVK, higher stability of the analytes in the medium and application of aqueous inorganic standards for calibration. The limits of detection for calcium, magnesium and zinc were 1.3 μg g(-1), 0.052 μg g(-1) and 0.41 μg g(-1), respectively. Concentrations of calcium, magnesium and zinc in six different samples obtained by the developed method did not differ significantly from the results obtained by the reference methods at the 95% confidence level (Student's t-test and ANOVA). Therefore, the proposed method becomes an efficient alternative for determination of metals in lubricating oil.

  20. UV-photochemical vapor generation of selenium for atomic absorption spectrometry: Optimization and 75Se radiotracer efficiency study

    NASA Astrophysics Data System (ADS)

    Rybínová, Marcela; Musil, Stanislav; Červený, Václav; Vobecký, Miloslav; Rychlovský, Petr

    2016-09-01

    Volatile selenium compounds were generated UV-photochemically in the continuous flow mode using four UV-photoreactors differing in the material of the reaction coil; Teflon tubing and quartz tubes with various inner diameters and wall thicknesses were tested. Atomic absorption spectrometry with an externally heated quartz furnace atomizer was employed as the detector. The relevant experimental generation parameters were optimized and the basic analytical characteristics were determined. Using formic acid as the photochemical agent, limits of detection achieved for selenium were in the range 46-102 ng L- 1 in dependence on the type of UV-photoreactor employed. When nitric acid was also added to the photochemical agent, the limits of detection were reduced to 27-44 ng L- 1. The repeatability did not exceed 2.4% (5 μg L- 1 Se(IV), n = 10). Experiments with 75Se radiotracer have been performed for the first time to quantify the efficiency of UV-photochemical vapor generation (UV-PVG) of selenium. The highest efficiency of 67 ± 1% was obtained for a UV-photoreactor containing a quartz reaction coil (2.0 mm i.d., 4.0 mm o.d.). The generation efficiency of 61 ± 1% was obtained for a Teflon reaction coil (1.0 mm i.d., 1.4 mm o.d.). Mapping of the radiotracer distribution in the individual parts of the apparatus did not reveal substantial transport losses of the analyte in the UV-PVG system.

  1. Tunable diode laser measurements of HO2NO2 absorption coefficients near 12.5 microns

    NASA Technical Reports Server (NTRS)

    May, R. D.; Molina, L. T.; Webster, C. R.

    1988-01-01

    A tunable diode laser spectrometer has been used to measure absorption coefficients of peroxynitric acid (HO2NO2) near the 803/cm Q branch. HO2NO2 concentrations in a low-pressure flowing gas mixture were determined from chemical titration procedures and UV absorption spectroscopy. The diode laser measured absorption coefficients, at a spectral resolution of better than 0.001/cm, are about 10 percent larger than previous Fourier transform infrared measurements made at a spectral resolution of 0.06/cm.

  2. Modified Sagnac interferometer for contact-free length measurement of a direct absorption cell.

    PubMed

    Elandaloussi, Hadj; Rouillé, Christian; Marie-Jeanne, Patrick; Janssen, Christof

    2016-03-10

    Accurate path length measurements in absorption cells are recurrent requirements in quantitative molecular absorption spectroscopy. A new twin path laser interferometer for length measurements in a simple direct path absorption geometry is presented, along with a full uncertainty budget. The path in an absorption cell is determined by measuring the optical path length change due to the diminution of the refractive index when the cell originally filled with nitrogen gas is evacuated. The performance of the instrument based on a stabilized HeNe laser is verified by comparison with the results of direct mechanical length measurements of a roughly 45 mm long, specially designed absorption cell. Due to a resolution of about 1/300 of a HeNe fringe, an expanded (coverage factor k=2) uncertainty of 16 μm in the length measurement is achieved, providing an expanded relative uncertainty of 3.6·10⁻⁴ for the length of our test absorption cell. This value is about 8 times lower than what has been reported previously. The instrument will be useful for precision measurements of absorption cross sections of strong absorbers which require short light paths, such as ozone, halogen oxides, sulfur dioxide, and volatile organic compounds in the UV.

  3. Quantitative infrared absorption cross sections of isoprene for atmospheric measurements

    SciTech Connect

    Brauer, Carolyn S.; Blake, Thomas A.; Guenther, Alex B.; Sharpe, Steven W.; Sams, Robert L.; Johnson, Timothy J.

    2014-11-19

    The OH- and O3- initiated oxidations of isoprene, which is one of the primary volatile organic compounds produced by vegetation, are a major source of atmospheric formaldehyde and other oxygenated organics, yet little quantitative IR data exists for isoprene. We thus report absorption coefficients and integrated band intensities for isoprene in the 600 - 6500 cm-1 region. The pressure-broadened (1 atmosphere N2) spectra were recorded at 278, 298 and 323 K in a 19.96 cm path length cell at 0.112 cm-1 resolution, using a Bruker 66V FTIR. Composite spectra are derived from a minimum of seven pressures at each temperature.

  4. Using broadband absorption spectroscopy to measure concentration of sulfur dioxide

    NASA Astrophysics Data System (ADS)

    Wang, H. S.; Zhang, Y. G.; Wu, S. H.; Lou, X. T.; Zhang, Z. G.; Qin, Y. K.

    2010-09-01

    A linear relationship between concentration of sulfur dioxide (SO2) and optical parameter (OP) is established using the Beer-Lambert law. The SO2 measuring system is set up to measure the concentration of sulfur dioxide in the wavelength range 275-315 nm. Experimental results indicate that the detection limit of the sulfur dioxide measuring system is below 0.2 ppm per meter of path length, and the measurement precision is better than ±1%. The proposed SO2 measuring method features limited interference from other gases and dust, and high stability and short response time.

  5. Comparison of two methods for blood lead analysis in cattle: graphite-furnace atomic absorption spectrometry and LeadCare(R) II system.

    PubMed

    Bischoff, Karyn; Gaskill, Cynthia; Erb, Hollis N; Ebel, Joseph G; Hillebrandt, Joseph

    2010-09-01

    The current study compared the LeadCare(R) II test kit system with graphite-furnace atomic absorption spectrometry for blood lead (Pb) analysis in 56 cattle accidentally exposed to Pb in the field. Blood Pb concentrations were determined by LeadCare II within 4 hr of collection and after 72 hr of refrigeration. Blood Pb concentrations were determined by atomic absorption spectrometry, and samples that were coagulated (n = 12) were homogenized before analysis. There was strong rank correlation (R(2) = 0.96) between atomic absorption and LeadCare II (within 4 hr of collection), and a conversion formula was determined for values within the observed range (3-91 mcg/dl, although few had values >40 mcg/dl). Median and mean blood pb concentrations for atomic absorption were 7.7 and 15.9 mcg/dl, respectively; for LeadCare II, medians were 5.2 mcg/dl at 4 hr and 4.9 mcg/dl at 72 hr, and means were 12.4 and 11.7, respectively. LeadCare II results at 4 hr strongly correlated with 72 hr results (R(2) = 0.96), but results at 72 hr were lower (P < 0.01). There was no significant difference between coagulated and uncoagulated samples run by atomic absorption. Although there have been several articles that compared LeadCare with other analytical techniques, all were for the original system, not LeadCare II. The present study indicated that LeadCare II results correlated well with atomic absorption over a wide range of blood Pb concentrations and that refrigerating samples for up to 72 hr before LeadCare II analysis was acceptable for clinical purposes.

  6. Cyclotron-absorption measurement of the runaway-electron distribution in a tokamak

    SciTech Connect

    Zvonkov, A.V.; Suvorov, E.V.; Timofeev, A.V.; Fraiman, A.A.

    1983-03-01

    The distribution function of runaway electrons in a tokamak can be determined in the slightly relativistic region from measurements of the absorption coefficient corresponding to electron cyclotron waves. The plasma should be probed in the vertical direction.

  7. Measurement of atmospheric precipitable water using a solar radiometer. [water vapor absorption effects

    NASA Technical Reports Server (NTRS)

    Pitts, D. E.; Dillinger, A. E.; Mcallum, W. E.

    1974-01-01

    A technique is described and tested that allows the determination of atmospheric precipitable water from two measurements of solar intensity: one in a water-vapor absorption band and another in a nearby spectral region unaffected by water vapor.

  8. Decay Heat Measurements Using Total Absorption Gamma-ray Spectroscopy

    NASA Astrophysics Data System (ADS)

    Rice, S.; Valencia, E.; Algora, A.; Taín, J. L.; Regan, P. H.; Podolyák, Z.; Agramunt, J.; Gelletly, W.; Nichols, A. L.

    2012-09-01

    A knowledge of the decay heat emitted by thermal neutron-irradiated nuclear fuel is an important factor in ensuring safe reactor design and operation, spent fuel removal from the core, and subsequent storage prior to and after reprocessing, and waste disposal. Decay heat can be readily calculated from the nuclear decay properties of the fission products, actinides and their decay products as generated within the irradiated fuel. Much of the information comes from experiments performed with HPGe detectors, which often underestimate the beta feeding to states at high excitation energies. This inability to detect high-energy gamma emissions effectively results in the derivation of decay schemes that suffer from the pandemonium effect, although such a serious problem can be avoided through application of total absorption γ-ray spectroscopy (TAS). The beta decay of key radionuclei produced as a consequence of the neutron-induced fission of 235U and 239Pu are being re-assessed by means of this spectroscopic technique. A brief synopsis is given of the Valencia-Surrey (BaF2) TAS detector, and their method of operation, calibration and spectral analysis.

  9. Quantitative infrared absorption cross sections of isoprene for atmospheric measurements

    DOE PAGES

    Brauer, C. S.; Blake, T. A.; Guenther, A. B.; ...

    2014-11-19

    Isoprene (C5H8, 2-methyl-1,3-butadiene) is a volatile organic compound (VOC) and is one of the primary contributors to annual global VOC emissions. Isoprene is produced primarily by vegetation as well as anthropogenic sources, and its OH- and O3-initiated oxidations are a major source of atmospheric oxygenated organics. Few quantitative infrared studies have been reported for isoprene, limiting the ability to quantify isoprene emissions via remote or in situ infrared detection. We thus report absorption cross sections and integrated band intensities for isoprene in the 600–6500 cm-1 region. The pressure-broadened (1 atmosphere N2) spectra were recorded at 278, 298, and 323 Kmore » in a 19.94 cm path-length cell at 0.112 cm-1 resolution, using a Bruker IFS 66v/S Fourier transform infrared (FTIR) spectrometer. Composite spectra are derived from a minimum of seven isoprene sample pressures, each at one of three temperatures, and the number densities are normalized to 296 K and 1 atm.« less

  10. Shock tube measurements of the optical absorption of triatomic carbon, C3

    NASA Technical Reports Server (NTRS)

    Jones, J. J.

    1977-01-01

    The spectral absorption of C3 has been measured in a shock tube using a test gas mixture of acetylene diluted with argon. The absorption of a pulsed xenon light source was measured by means of eight photomultiplier channels to a spectrograph and an accompanying drum camera. The postshock test gas temperature and pressure were varied over the range 3300-4300 K and 0.36 to 2.13 atmospheres, respectively. The results showed appreciable absorption from C3 for the wavelength range 300 to 540 nanometers. The computed electronic oscillator strength varied from 0.12 to 0.06 as a function of temperature.

  11. Absorption measurement of thin films by using photothermal techniques: The influence of thermal properties

    SciTech Connect

    Wu, Z.L.; Kuo, P.K.; Thomas, R.L.; Fan, Z.X.

    1995-12-31

    Photothermal techniques are widely used for measuring optical absorption of thin film coatings. In these applications the calibration of photothermal signal is typically based on the assumption that the thermal properties of the thin film make very little contribution. In this paper we take mirage technique as an example and present a detailed analysis of the influence of thin film thermal properties on absorption measurements. The results show that the traditional calibration method is not valid on surprisingly many situations.

  12. Temperature measurement using ultraviolet laser absorption of carbon dioxide behind shock waves.

    PubMed

    Oehlschlaeger, Matthew A; Davidson, David F; Jeffries, Jay B

    2005-11-01

    A diagnostic for microsecond time-resolved temperature measurements behind shock waves, using ultraviolet laser absorption of vibrationally hot carbon dioxide, is demonstrated. Continuous-wave laser radiation at 244 and 266 nm was employed to probe the spectrally smooth CO2 ultraviolet absorption, and an absorbance ratio technique was used to determine temperature. Measurements behind shock waves in both nonreacting and reacting (ignition) systems were made, and comparisons with isentropic and constant-volume calculations are reported.

  13. Intestinal adaptation in patients with short bowel syndrome. Measurement by calcium absorption

    SciTech Connect

    Gouttebel, M.C.; Saint Aubert, B.; Colette, C.; Astre, C.; Monnier, L.H.; Joyeux, H. )

    1989-05-01

    Functional adaptation of remaining intestine was evaluated in 30 patients with extensive small bowel resection. Calcium and xylose absorption tests were compared. Calcium absorption was measured by a double-radiotracer technique. Serum xylosemia was measured 2 hr after D-xylose ingestion. Patients were divided into two groups according to the time interval between surgery and evaluation: less (group I) or more (group II) than two years. A statistically significant correlation was found between xylosemia and remaining small bowel length (r = 0.71; P less than 0.001) and between calcium absorption and remaining small bowel length (r = 0.75; P less than 0.001) in group I. A significant correlation was also observed between calcium absorption and time after surgery (r = 0.65; P = 0.001) but not for xylose absorption. Calcium absorption value was significantly increased in group II patients compared with group I patients matched for remaining small bowel length (36.2 +/- 12.5% vs 14.5 +/- 9.1%; P less than 0.001) while no difference was observed between the two groups concerning xylose absorption. These data indicate that intestinal calcium absorption continues to increase for more than two years after a major bowel resection in man. The intestine does not seem to recover all its functions at the same time.

  14. Monitoring complex trace-gas mixtures by long-path laser absorption spectrometry. [in long duration manned mission closed environments

    NASA Technical Reports Server (NTRS)

    Green, B. D.; Steinfeld, J. I.

    1976-01-01

    Laser-based spectrophotometric methods, which have been proposed for the detection of trace concentrations of gaseous contaminants, include Raman and passive radiometry. The paper discusses a simple long-path laser absorption method which is capable of resolving complex mixtures of closely related trace contaminants at ppm levels. A number of species were selected which are most likely to accumulate in closed environments, such as submarines or long-duration manned space flights. Absorption coefficients at CO2 laser wavelengths were measured, accurate to + 3 per cent or better, for each of these species. This data base was then used to determine the presence and concentration of the contaminants in prepared mixtures of 12 to 15 gases. Computer programs have been developed which will permit a real-time analysis of the monitored atmosphere. Minimum detectable concentrations for individual species are generally in the ppm range, and are not seriously degraded by interferences even in complex mixtures. Estimates of the dynamic range of this monitoring technique for various system configurations and comparison with other methods of analysis are discussed

  15. Measurements of Soot Mass Absorption Coefficients from 300 to 660 nm

    NASA Astrophysics Data System (ADS)

    Renbaum-Wolff, Lindsay; Fisher, Al; Helgestad, Taylor; Lambe, Andrew; Sedlacek, Arthur; Smith, Geoffrey; Cappa, Christopher; Davidovits, Paul; Onasch, Timothy; Freedman, Andrew

    2016-04-01

    Soot, a product of incomplete combustion, plays an important role in the earth's climate system through the absorption and scattering of solar radiation. In particular, the assumed mass absorption coefficient (MAC) of soot and its variation with wavelength presents a significant uncertainty in the calculation of radiative forcing in global climate change models. As part of the fourth Boston College/Aerodyne soot properties measurement campaign, we have measured the mass absorption coefficient of soot produced by an inverted methane diffusion flame over a spectral range of 300-660 nm using a variety of optical absorption techniques. Extinction and absorption were measured using a dual cavity ringdown photoacoustic spectrometer (CRD-PAS, UC Davis) at 405 nm and 532 nm. Scattering and extinction were measured using a CAPS PMssa single scattering albedo monitor (Aerodyne) at 630 nm; the absorption coefficient was determined by subtraction. In addition, the absorption coefficients in 8 wavelength bands from 300 to 660 nm were measured using a new broadband photoacoustic absorption monitor (UGA). Soot particle mass was quantified using a centrifugal particle mass analyzer (CPMA, Cambustion), mobility size with a scanning mobility particle sizer (SMPS, TSI) and soot concentration with a CPC (Brechtel). The contribution of doubly charged particles to the sample mass was determined using a Single Particle Soot Photometer (DMT). Over a mass range of 1-8 fg, corresponding to differential mobility diameters of ~150 nm to 550 nm, the value of the soot MAC proved to be independent of mass for all wavelengths. The wavelength dependence of the MAC was best fit to a power law with an Absorption Ångstrom Coefficient slightly greater than 1.

  16. Mass specific optical absorption coefficients of mineral dust components measured by a multi wavelength photoacoustic spectrometer

    NASA Astrophysics Data System (ADS)

    Utry, N.; Ajtai, T.; Pintér, M.; Tombácz, E.; Illés, E.; Bozóki, Z.; Szabó, G.

    2014-09-01

    Mass specific optical absorption coefficients of various mineral dust components including silicate clays (illite, kaolin and bentonite), oxides (quartz, hematite and rutile), and carbonate (limestone) were determined at wavelengths of 1064, 532, 355 and 266 nm. These values were calculated from aerosol optical absorption coefficients measured by a multi-wavelength photoacoustic (PA) instrument, the mass concentration and the number size distribution of the generated aerosol samples as well as the size transfer functions of the measuring instruments. These results are expected to have considerable importance in global radiative forcing calculations. They can also serve as reference for validating calculated wavelength dependent imaginary parts (κ) of complex refractive indices which up to now have been typically deduced from bulk phase measurements by using indirect measurement methods. Accordingly, the presented comparison of the measured and calculated aerosol optical absorption spectra revealed the strong need for standardized sample preparation and measurement methodology in case of bulk phase measurements.

  17. Minute Concentration Measurements of Simple Hydrocarbon Species Using Supercontinuum Laser Absorption Spectroscopy.

    PubMed

    Yoo, Jihyung; Traina, Nicholas; Halloran, Michael; Lee, Tonghun

    2016-06-01

    Minute concentration measurements of simple hydrocarbon gases are demonstrated using near-infrared supercontinuum laser absorption spectroscopy. Absorption-based gas sensors, particularly when combined with optical fiber components, can significantly enhance diagnostic capabilities to unprecedented levels. However, these diagnostic techniques are subject to limitations under certain gas sensing applications where interference and harsh conditions dominate. Supercontinuum laser absorption spectroscopy is a novel laser-based diagnostic technique that can exceed the above-mentioned limitations and provide accurate and quantitative concentration measurement of simple hydrocarbon species while maintaining compatibility with telecommunications-grade optical fiber components. Supercontinuum radiation generated using a highly nonlinear photonic crystal fiber is used to probe rovibrational absorption bands of four hydrocarbon species using full-spectral absorption diagnostics. Absorption spectra of methane (CH4), acetylene (C2H2), and ethylene (C2H4) were measured in the near-infrared spectrum at various pressures and concentrations to determine the accuracy and feasibility of the diagnostic strategy. Absorption spectra of propane (C3H8) were subsequently probed between 1650 nm and 1700 nm, to demonstrate the applicability of the strategy. Measurements agreed very well with simulated spectra generated using the HITRAN database as well as with previous experimental results. Absorption spectra of CH4, C2H2, and C2H4 were then analyzed to determine their respective measurement accuracy and detection limit. Concentration measurements integrated from experimental results were in very good agreement with independent concentration measurements. Calculated detection limits of CH4, C2H2, and C2H4 at room temperature and atmospheric pressure are 0.1%, 0.09%, and 0.17%, respectively.

  18. A novel analytical system involving hydride generation and gold-coated W-coil trapping atomic absorption spectrometry for selenium determination at ng l - 1 level

    NASA Astrophysics Data System (ADS)

    Kula, İ.; Arslan, Y.; Bakırdere, S.; Ataman, O. Y.

    2008-08-01

    A novel analytical technique was developed where gaseous hydrogen selenide formed by sodium tetrahydroborate reduction is transported to and trapped on a resistively heated gold-coated W-coil atom trap for in situ preconcentration. Gold coating on W-coil was prepared by using an organic solution of Au. The atom trap is held at 165 °C during the collection stage and is heated up to 675 °C for revolatilization; analyte species formed are transported to an externally heated quartz T-tube where the atomization takes place and the transient signal is obtained. The carrier gas consisted of 112.5 ml min - 1 Ar with 75 ml min - 1 H 2 during the collection step and 112.5 ml min - 1 Ar with 450 ml min - 1 H 2 in the revolatilization step. The half width of the transient signal obtained is less than 0.5 s. The RSD for the measurements was found to be 3.9% ( n = 11) for 0.10 µg l - 1 Se using peak height measurements. The calibration plot for 27.0 ml of sample collected in 4.0 min using a flow rate of 6.75 ml min - 1 was linear between 0.13 and 2.0 µg l - 1 of Se. The limit of detection (3 s) is 39 ng l - 1 . The enhancement factor for the characteristic concentration ( Co) was found to be 20.1 when compared to conventional hydride generation atomic absorption spectrometry system without trap. In order to check the accuracy of the method, standard reference material, natural water NIST 1640 was employed; the result was found to be in good agreement with the certified value at the 95% confidence level.

  19. Speciation and determination of ultra trace amounts of inorganic tellurium in environmental water samples by dispersive liquid-liquid microextraction and electrothermal atomic absorption spectrometry.

    PubMed

    Najafi, Nahid Mashkouri; Tavakoli, Hamed; Alizadeh, Reza; Seidi, Shahram

    2010-06-18

    A simple and powerful method has been developed for the rapid and selective determination of Te(IV) and Te(VI), employing dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry using palladium as permanent modifier. Under acidic conditions pH 1, only Te(IV) can form a complex with ammonium pyrrolidine dithiocarbamate (APDC) and therefore be extracted into fine droplets of carbon tetrachloride (extraction solvent) which are dispersed with ethanol into the water sample solution. After centrifugation, Te(IV) was determined in the sedimented organic phase while Te(VI) remained in the aqueous phase. Total inorganic tellurium was determined after the reduction of the Te(VI) to Te(IV). Te(VI) was calculated as the difference between the measured total inorganic tellurium and Te(IV) content. The effective parameters for improving the efficiency of microextraction process were investigated by using experimental and central composite designs. Under optimal conditions the enrichment factor was 125 and the calibration graph was linear in the range of 0.015-1 ng mL(-1) with detection limit and characteristic mass of 0.004 ng mL(-1) and 0.033 pg, respectively. The relative standard deviation for 0.5 ng mL(-1) of tellurium measurement was 3.6% (n=6) at ash and atomization temperature, 900 and 2600 degrees C, respectively. The recoveries of spiked Te(IV) and Te(VI) to the environmental water samples were 89.6-101.3% and 96.6-99.1%, respectively. The accuracy is also evaluated by applying the proposed method to certified reference material (NIST SRM 1643e), for which the result was in a good agreement with the certified values reported for this CRM (95% confidence level).

  20. Measurement of Carbon Dioxide Column via Space Borne Laser Absorption

    NASA Technical Reports Server (NTRS)

    Heaps, WIlliam S.

    2007-01-01

    In order to better understand the budget of carbon dioxide in the Earth's atmosphere it is necessary to develop a global high precision understanding of the carbon dioxide column. In order to uncover the 'missing sink that is responsible for the large discrepancies in the budget as we presently understand it calculation has indicated that measurement accuracy on the order of 1 ppm is necessary. Because typical column average CO2 has now reached 380 ppm this represents a precision on the order of .25% for these column measurements. No species has ever been measured from space at such a precision. In recognition of the importance of understanding the CO2 budget in order to evaluate its impact on global warming the National Research Council in its decadal survey report to NASA recommended planning for a laser based total CO2 mapping mission in the near future. The extreme measurement accuracy requirements on this mission places very strong requirements on the laser system used for the measurement. This work presents an analysis of the characteristics necessary in a laser system used to make this measurement. Consideration is given to the temperature dependence, pressure broadening, and pressure shift of the CO2 lines themselves and how these impact the laser system characteristics Several systems for meeting these requirements that are under investigation at various institutions in the US as well as Europe will be discussed.

  1. Determination of trace elements in coal and coal fly ash by joint-use of ICP-AES and atomic absorption spectrometry.

    PubMed

    Iwashita, Akira; Nakajima, Tsunenori; Takanashi, Hirokazu; Ohki, Akira; Fujita, Yoshio; Yamashita, Toru

    2007-01-15

    Microwave-acid digestion (MW-AD) followed by inductively coupled plasma-atomic emission spectrometry (ICP-AES), graphite furnace atomic absorption spectrometry (GFAAS), and hydride generation atomic absorption spectrometry (HGAAS) were examined for the determination of various elements in coal and coal fly ash (CFA). Eight certified reference materials (four coal samples and four CFA samples) were tested. The 10 elements (As, Be, Cd, Co, Cr, Mn, Ni, Pb, Sb, and Se), which are described in the Clean Air Act Amendments (CAAA), were especially considered. For coal, the HF-free MW-AD followed by ICP-AES was successful in the determination of various elements except for As, Be, Cd, Sb, and Se. These elements (except for Sb) were well-determined by use of GFAAS (Be and Cd) and HGAAS (As and Se). For CFA, the addition of HF in the digestion acid mixture was needed for the determination of elements, except for As, Sb, and Se, for which the HF-free MW-AD was applicable. The use of GFAAS (Be and Cd) or HGAAS (Sb and Se) resulted in the successful determination of the elements for which ICP-AES did not work well. The protocol for the determination of the 10 elements in coal and CFA by MW-AD followed by the joint-use of ICP-AES, GFAAS, and HGAAS was established.

  2. Measurement of Two-Photon Absorption Cross Section of Metal Ions by a Mass Sedimentation Approach

    PubMed Central

    Ma, Zhuo-Chen; Chen, Qi-Dai; Han, Bing; Liu, Xue-Qing; Song, Jun-Feng; Sun, Hong-Bo

    2015-01-01

    The photo-reduction of metal ions in solution induced by femtosecond laser is an important and novel method for fabricating three-dimensional metal microstructures. However, the nonlinear absorption cross section of metal ions remains unknown because its measurement is difficult. In the present study, a method based on Two-Photon Excited Sedimentation (TPES) is proposed to measure the two-photon absorption cross section (TPACS) of metal ions in solution. The power-squared dependence of the amount of sediment on the excitation intensity was confirmed, revealing that 800 nm femtosecond laser induced reduction of metal ions was a two photon absorption process. We believe that the proposed method may be applied to measure the TPACS of several metal ions, thereby opening a new avenue towards future analysis of two-photon absorption materials. PMID:26657990

  3. Method and apparatus for background signal reduction in opto-acoustic absorption measurement

    NASA Technical Reports Server (NTRS)

    Rosengren, L. G. (Inventor)

    1976-01-01

    The sensitivity of an opto-acoustic absorption detector is increased to make it possible to measure trace amounts of constituent gases. A second beam radiation path is created through the sample cell identical to a first path except as to length, alternating the beam through the two paths and minimizing the detected pressure difference for the two paths while the beam wavelength is tuned away from the absorption lines of the sample. Then with the beam wavelength tuned to the absorption line of any constituent of interest, the pressure difference is a measure of trace amounts of the constituent. The same improved detector may also be used for measuring the absorption coefficient of known concentrations of absorbing gases.

  4. Re-Evaluation of Dust Radiative Forcing Using Remote Measurements of Dust Absorption

    NASA Technical Reports Server (NTRS)

    Kaufman, Yoram J.; Tanre, Didier; Karnieli, Arnon; Remer, Lorraine A.

    1998-01-01

    Spectral remote observations of dust properties from space and from the ground creates a powerful tool for determination of dust absorption of solar radiation with an unprecedented accuracy. Absorption is a key component in understanding dust impact on climate. We use Landsat spaceborne measurements at 0.47 to 2.2 microns over Senegal with ground based sunphotometers to find that Saharan dust absorption of solar radiation is two to four times smaller than in models. Though dust absorbs in the blue, almost no absorption was found for wavelengths greater 0.6 microns. The new finding increases by 50% recent estimated solar radiative forcing by dust and decreases the estimated dust heating of the lower troposphere. Dust transported from Asia shows slightly higher absorption probably due to the presence of black carbon from populated regions. Large scale application of this method to satellite data from the Earth Observing System can reduce significantly the uncertainty in the dust radiative effects.

  5. Effect of magnesium acetylacetonate on the signal of organic forms of vanadium in graphite furnace atomic absorption spectrometry.

    PubMed

    Kowalewska, Zofia; Welz, Bernhard; Castilho, Ivan N B; Carasek, Eduardo

    2013-01-15

    The aim of this work was to investigate the influence of magnesium acetylacetonate (MgA) on the signal of organic forms of vanadium in xylene solution by graphite furnace atomic absorption spectrometry. MgA alone or mixed with palladium acetylacetonate (PdA) was considered as a chemical modifier. It has been found that MgA does not improve, but decreases significantly the integrated absorbance of V in the form of alkyl-aryl sulfonates, acetylacetonates, porphyrins and in lubricating oils, while its effect is negligible in the case of "dark products" from petroleum distillation, i.e., heavy oil fractions and residues. The decrease is also observed in the presence of Pd. The MgA (or MgA+PdA) effect on the integrated absorbance of V has been studied using the following variants: different ways of modifier application, various pyrolysis temperature, additional application of air ashing, preliminary pretreatment with iodine and methyltrioctylammonium chloride, application of various graphite furnace heating systems (longitudinal or transverse) and various optical and background correction systems (medium-resolution line source spectrometer with deuterium background correction or high-resolution continuum source spectrometer). The experiments indicate formation of more refractory compounds as a possible reason for the decrease of the integrated absorbance for some forms of V in the presence of MgA. The application of MgA as a chemical modifier in V determination is not recommended. Results of this work have general importance as, apart from the intentional use of MgA as a modifier, organic Mg compounds, present in petroleum products for other reason (e.g. as an additive), can influence the signal of V compounds and hence the accuracy in V determination. Generally, petroleum products with known amount of V are recommended as standards; however, lubricating oils can be inadequate for "dark products" from petroleum distillation. In the case of unknown samples it is

  6. Simultaneous determination of cadmium, iron and tin in canned foods using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

    Leao, Danilo J; Junior, Mario M S; Brandao, Geovani C; Ferreira, Sergio L C

    2016-06-01

    A method was established to simultaneously determine cadmium, iron and tin in canned-food samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). The quantification step has been performed using the primary line (228.802nm) for cadmium and the adjacent secondary lines (228.725nm and 228.668nm) for iron and tin, respectively. The selected chemical modifier was an acid solution that contained a mixture of 0.1% (w/v) Pd and 0.05% (w/v) Mg. The absorbance signals were measured based on the peak area using 3 pixels for cadmium and 5 pixels for iron and tin. Under these conditions, cadmium, iron and tin have been determined in canned-food samples using the external calibration technique based on aqueous standards, where the limits of quantification were 2.10ngg(-1) for cadmium, 1.95mgkg(-1) for iron and 3.00mgkg(-1) for tin, and the characteristic masses were 1.0pg for cadmium, 0.9ng for iron and 1.1ng for tin. The precision was evaluated using two solutions of each metal ion, and the results, which were expressed as the relative standard deviation (RSD%), were 3.4-6.8%. The method accuracy for cadmium and iron was confirmed by analyzing a certified reference material of apple leaves (NIST 1515), which was supplied by NIST. However, for tin, the accuracy was confirmed by comparing the results of the proposed method and another analytical technique (inductively coupled plasma optical emission spectrometry). The proposed procedure was applied to determine cadmium, iron and tin in canned samples of peeled tomato and sardine. Eleven samples were analyzed, and the analyte concentrations were 3.57-62.9ngg(-1), 2.68-31.48mgkg(-1) and 4.06-122.0mgkg(-1) for cadmium, iron and tin, respectively. In all analyzed samples, the cadmium and tin contents were lower than the permissible maximum levels for these metals in canned foods in the Brazilian legislation.

  7. Method for measuring changes in light absorption of highly scattering media

    DOEpatents

    Bigio, Irving J.; Johnson, Tamara M.; Mourant, Judith R.

    2002-01-01

    The noninvasive measurement of variations in absorption that are due to changes in concentrations of biochemically relevant compounds in tissue is important in many clinical settings. One problem with such measurements is that the pathlength traveled by the collected light through the tissue depends on the scattering properties of the tissue. It is demonstrated, using both Monte Carlo simulations and experimental measurements, that for an appropriate separation between light-delivery and light-collection fibers, the pathlength of the collected photons is insensitive to scattering parameters for the range of parameters typically found in tissue. This is important for developing rapid, noninvasive, inexpensive, and accurate methods for measuring absorption changes in tissue.

  8. In vivo low-coherence spectroscopic measurements of local hemoglobin absorption spectra in human skin

    NASA Astrophysics Data System (ADS)

    Bosschaart, Nienke; Faber, Dirk J.; van Leeuwen, Ton G.; Aalders, Maurice C. G.

    2011-10-01

    Localized spectroscopic measurements of optical properties are invaluable for diagnostic applications that involve layered tissue structures, but conventional spectroscopic techniques lack exact control over the size and depth of the probed tissue volume. We show that low-coherence spectroscopy (LCS) overcomes these limitations by measuring local attenuation and absorption coefficient spectra in layered phantoms. In addition, we demonstrate the first in vivo LCS measurements of the human epidermis and dermis only. From the measured absorption in two distinct regions of the dermal microcirculation, we determine total hemoglobin concentration (3.0+/-0.5 g/l and 7.8+/-1.2 g/l) and oxygen saturation.

  9. In vivo low-coherence spectroscopic measurements of local hemoglobin absorption spectra in human skin.

    PubMed

    Bosschaart, Nienke; Faber, Dirk J; van Leeuwen, Ton G; Aalders, Maurice C G

    2011-10-01

    Localized spectroscopic measurements of optical properties are invaluable for diagnostic applications that involve layered tissue structures, but conventional spectroscopic techniques lack exact control over the size and depth of the probed tissue volume. We show that low-coherence spectroscopy (LCS) overcomes these limitations by measuring local attenuation and absorption coefficient spectra in layered phantoms. In addition, we demonstrate the first in vivo LCS measurements of the human epidermis and dermis only. From the measured absorption in two distinct regions of the dermal microcirculation, we determine total hemoglobin concentration (3.0±0.5 g∕l and 7.8±1.2 g∕l) and oxygen saturation.

  10. In Situ Measurements of Aerosol Mass Concentration and Spectral Absorption in Xianghe, SE of Beijing, China

    NASA Astrophysics Data System (ADS)

    Chaudhry, Z.; Martins, V.; Li, Z.

    2005-12-01

    China's rapid industrialization over the last few decades has affected air quality in many regions of China, and even the regional climate. As a part of the EAST-AIRE (East Asian Study of Tropospheric Aerosols: an International Regional Experiment) study, Nuclepore filters were collected in two size ranges (PM10 and PM2.5) at 12 hour intervals since January 2005 at Xianghe, about 70 km southeast of Beijing. Each filter was analyzed for mass concentration, aerosol scattering and absorption efficiencies. Mass concentrations during the winter months (January-March) ranged from 9 to 459 μg/m3 in the coarse mode with an average concentration of 122 μg/m3, and from 11 to 203 μg/m3 in the fine mode with an average concentration of 45 μg/m3. While some of the extreme values are likely linked to local emissions, regional air pollution episodes also played important roles. Absorption efficiency measurements at 550 nm show very high values compared to measurements performed in the United States during the CLAMS experiment. The spectral mass absorption efficiency was measured from 350 to 2500 nm and shows large differences between the absorption properties of soil dust, black carbon, and organic aerosols. The strong spectral differences observed can be related to differences in refractive indices from the several collected species and particle size effects. The absorption properties from aerosols measured in China show large absorption efficiencies, compared to aerosols measured in the US, possibly linked to different technology practices used in these countries. For organic plus black carbon aerosols, where the refractive index seems to be relatively constant, the absorption efficiency spectral dependence for fine mode aerosols falls between 1/λ and 1/λ2. The coarse mode absorption shows much less spectral dependence.

  11. Instrumentation for Combined Dispersion and Absorption Measurements in the VUV.

    PubMed

    Banfield, F P; Huber, M C; Parkinson, W H; Tubbs, E F

    1973-06-01

    When the hook method that measures anomalous dispersion is combined with photoelectric photometry, a particularly powerful tool results. An apparatus that combines these techniques over a wavelength range extending into the vacuum ultraviolet has been constructed and used chiefly on the iron-group elements. It consists of hydrogen-discharge light source, a Mach-Zehnder interferormeter, a high temperature furnace, a stigmatic spectrograph, and a photoelectric photometer.

  12. Assessment of multiphoton absorption in inert gases for the measurement of gas temperatures.

    PubMed

    Bednar, Natalie J; Walewski, Joachim W; Sanders, Scott T

    2006-03-01

    A spatially resolved optical technique to measure gas temperature was assessed. The technique relies on multiphoton absorption in inert gases. In contrast to laser-induced fluorescence, absorption is insensitive to collisional deactivation, and, in contrast to one-photon absorption, multiphoton absorption only occurs around the focus point of a typical laser beam. Multiphoton absorption features both the merits of being insensitive to quenching and of being a spatially resolved technique. In a case study we assessed two-photon absorption in xenon upon exciting the 5p6 1S0-->5p56p[5/2]2 transition in xenon at a wavelength of 256 nm. The amount of light absorbed by xenon is related to the number density of the gas, and if the gas pressure is known then the gas temperature can be inferred from the number density. Two-photon absorbance was measured as a function of xenon number density and was used to validate a theoretical model of the absorption process. We discuss the circumnavigation of experimental challenges in applying this technique and analyze its precision in terms of the inferred gas temperature.

  13. [Determination of Al, Be, Cd, Co, Cr, Mn, Ni, Pb, Se and Tl in whole blood by atomic absorption spectrometry without preliminary sample digestion].

    PubMed

    Ivanenko, N B; Ivanenko, A A; Solov'ev, N D; Navolotskiĭ, D V; Pavlova, O V; Ganeev, A A

    2014-01-01

    Methods of whole blood trace element determination by Graphite furnace atomic absorption spectrometry (in the variant of Zeeman's modulation polarization spectrometry) have been proposed. They do not require preliminary sample digestion. Furnace programs, modifiers and blood dilution factors were optimized. Seronorm™ human whole blood reference materials were used for validation. Dynamic ranges (for undiluted blood samples) were: Al 8 ¸ 210 мg/L; Be 0.3 ¸ 50 мg/L; Cd 0.2 ¸ 75 мg/L; Сo 5 ¸ 350 мg/L; Cr 10 ¸ 100 мg/L; Mn 6 ¸ 250 мg/L; Ni 10 ¸ 350 мg/L; Pb 3 ¸ 240 мg/L; Se 10 ¸ 500 мg/L; Tl 2 ¸ 600 мg/L. Precision (RSD) for the middle of dynamic range ranged from 5% for Mn to 11 for Se.

  14. Microwave Resonator Measurements of Atmospheric Absorption Coefficients: A Preliminary Design Study

    NASA Technical Reports Server (NTRS)

    Walter, Steven J.; Spilker, Thomas R.

    1995-01-01

    A preliminary design study examined the feasibility of using microwave resonator measurements to improve the accuracy of atmospheric absorption coefficients and refractivity between 18 and 35 GHz. Increased accuracies would improve the capability of water vapor radiometers to correct for radio signal delays caused by Earth's atmosphere. Calibration of delays incurred by radio signals traversing the atmosphere has applications to both deep space tracking and planetary radio science experiments. Currently, the Cassini gravity wave search requires 0.8-1.0% absorption coefficient accuracy. This study examined current atmospheric absorption models and estimated that current model accuracy ranges from 5% to 7%. The refractivity of water vapor is known to 1% accuracy, while the refractivity of many dry gases (oxygen, nitrogen, etc.) are known to better than 0.1%. Improvements to the current generation of models will require that both the functional form and absolute absorption of the water vapor spectrum be calibrated and validated. Several laboratory techniques for measuring atmospheric absorption and refractivity were investigated, including absorption cells, single and multimode rectangular cavity resonators, and Fabry-Perot resonators. Semi-confocal Fabry-Perot resonators were shown to provide the most cost-effective and accurate method of measuring atmospheric gas refractivity. The need for accurate environmental measurement and control was also addressed. A preliminary design for the environmental control and measurement system was developed to aid in identifying significant design issues. The analysis indicated that overall measurement accuracy will be limited by measurement errors and imprecise control of the gas sample's thermodynamic state, thermal expansion and vibration- induced deformation of the resonator structure, and electronic measurement error. The central problem is to identify systematic errors because random errors can be reduced by averaging

  15. [Gas Concentration Measurement Based on the Integral Value of Absorptance Spectrum].

    PubMed

    Liu, Hui-jun; Tao, Shao-hua; Yang, Bing-chu; Deng, Hong-gui

    2015-12-01

    The absorptance spectrum of a gas is the basis for the qualitative and quantitative analysis of the gas by the law of the Lambert-Beer. The integral value of the absorptance spectrum is an important parameter to describe the characteristics of the gas absorption. Based on the measured absorptance spectrum of a gas, we collected the required data from the database of HIT-RAN, and chose one of the spectral lines and calculated the integral value of the absorptance spectrum in the frequency domain, and then substituted the integral value into Lambert-Beer's law to obtain the concentration of the detected gas. By calculating the integral value of the absorptance spectrum we can avoid the more complicated calculation of the spectral line function and a series of standard gases for calibration, so the gas concentration measurement will be simpler and faster. We studied the changing trends of the integral values of the absorptance spectrums versus temperature. Since temperature variation would cause the corresponding variation in pressure, we studied the changing trends of the integral values of the absorptance spectrums versus both the pressure not changed with temperature and changed with the temperature variation. Based on the two cases, we found that the integral values of the absorptance spectrums both would firstly increase, then decrease, and finally stabilize with temperature increasing, but the ranges of specific changing trend were different in the two cases. In the experiments, we found that the relative errors of the integrated values of the absorptance spectrum were much higher than 1% and still increased with temperature when we only considered the change of temperature and completely ignored the pressure affected by the temperature variation, and the relative errors of the integrated values of the absorptance spectrum were almost constant at about only 1% when we considered that the pressure were affected by the temperature variation. As the integral value

  16. Dynamics of laser-driven proton acceleration exhibited by measured laser absorptivity and reflectivity

    PubMed Central

    Bin, J. H.; Allinger, K.; Khrennikov, K.; Karsch, S.; Bolton, P. R.; Schreiber, J.

    2017-01-01

    Proton acceleration from nanometer thin foils with intense laser pulses is investigated experimentally. We analyzed the laser absorptivity by parallel monitoring of laser transmissivity and reflectivity with different laser intensities when moving the targets along the laser axis. A direct correlation between laser absorptivity and maximum proton energy is observed. Experimental results are interpreted in analytical estimation, exhibiting a coexistence of plasma expansion and light-sail form of radiation pressure acceleration (RPA-LS) mechanisms during the entire proton acceleration process based on the measured laser absorptivity and reflectivity. PMID:28272471

  17. Active feedback regulation of a Michelson interferometer to achieve zero-background absorption measurements.

    PubMed

    Lundin, Patrik; Guan, Zuguang; Svanberg, Sune

    2011-01-20

    An active phase-controlling scheme based on a proportional-integral-derivative-controlled piezoelectric transducer is presented with the purpose of stabilizing a quasi-zero-background absorption spectrometer. A fiber-based balanced Michelson interferometer is used, and absorption due to a gas sample in one of its arms results in an increased light signal to a detector, which otherwise, thanks to destructive interference, experiences a very low light level. With the presented approach, the sensitivity of already potent absorption measurement techniques, e.g., based on modulation, could be improved even further.

  18. Deriving brown carbon from multiwavelength absorption measurements: Method and application to AERONET and Aethalometer observations

    SciTech Connect

    Wang, X.; Heald, C. L.; Sedlacek, A.; de Sa, S. S.; Martin, S. T.; Alexander, M. L.; Watson, T. B.; Aiken, A. C.; Springston, S. R.; Artaxo, P.

    2016-10-13

    The radiative impact of organic aerosols (OA) is a large source of uncertainty in estimating the global direct radiative effect (DRE) of aerosols. This radiative impact includes not only light scattering but also light absorption from a subclass of OA referred to as brown carbon (BrC). However the absorption properties of BrC are poorly understood leading to large uncertainties in modelling studies. To obtain observational constraints from measurements, a simple Absorption Ångström Exponent (AAE) method is often used to separate the contribution of BrC absorption from that of black carbon (BC). However, this attribution method is based on assumptions regarding the spectral dependence of BC that are often violated in the ambient atmosphere. Here we develop a new method that decreases the uncertainties associated with estimating BrC absorption. By applying this method to multi-wavelength absorption aerosol optical depth (AAOD) measurements at AERONET sites worldwide and surface aerosol absorption measurements at multiple ambient sites, we estimate that BrC globally contributes 6-40% of the absorption at 440nm. We find that the mass absorption coefficient of OA (OA-MAC) is positively correlated with BC/OA mass ratio. Based on the variability of BC properties and BC/OA emission ratio, we estimate a range of 0.05-1.2 m2/g for OA-MAC at 440nm. Using the combination of AERONET and OMI UV absorption observations we estimate that the AAE388/440nm for BrC is generally ~4 world-wide, with a smaller value in Europe (< 2). Our analyses of two surface sites (Cape Cod, to the southeast of Boston, and the GoAmazon2014/5 T3 site, to the west of Manaus, Brazil) reveal no significant relationship between BrC absorptivity and photochemical aging in typical urban influenced conditions. However, the absorption of BrC measured during the biomass burning season near Manaus is found to decrease with photochemical aging with a lifetime of ~1 day. This lifetime is

  19. Deriving brown carbon from multiwavelength absorption measurements: Method and application to AERONET and Aethalometer observations

    DOE PAGES

    Wang, X.; Heald, C. L.; Sedlacek, A.; ...

    2016-10-13

    The radiative impact of organic aerosols (OA) is a large source of uncertainty in estimating the global direct radiative effect (DRE) of aerosols. This radiative impact includes not only light scattering but also light absorption from a subclass of OA referred to as brown carbon (BrC). However the absorption properties of BrC are poorly understood leading to large uncertainties in modelling studies. To obtain observational constraints from measurements, a simple Absorption Ångström Exponent (AAE) method is often used to separate the contribution of BrC absorption from that of black carbon (BC). However, this attribution method is based on assumptions regardingmore » the spectral dependence of BC that are often violated in the ambient atmosphere. Here we develop a new method that decreases the uncertainties associated with estimating BrC absorption. By applying this method to multi-wavelength absorption aerosol optical depth (AAOD) measurements at AERONET sites worldwide and surface aerosol absorption measurements at multiple ambient sites, we estimate that BrC globally contributes 6-40% of the absorption at 440nm. We find that the mass absorption coefficient of OA (OA-MAC) is positively correlated with BC/OA mass ratio. Based on the variability of BC properties and BC/OA emission ratio, we estimate a range of 0.05-1.2 m2/g for OA-MAC at 440nm. Using the combination of AERONET and OMI UV absorption observations we estimate that the AAE388/440nm for BrC is generally ~4 world-wide, with a smaller value in Europe (< 2). Our analyses of two surface sites (Cape Cod, to the southeast of Boston, and the GoAmazon2014/5 T3 site, to the west of Manaus, Brazil) reveal no significant relationship between BrC absorptivity and photochemical aging in typical urban influenced conditions. However, the absorption of BrC measured during the biomass burning season near Manaus is found to decrease with photochemical aging with a lifetime of ~1 day. This lifetime is comparable to

  20. Dynamics of laser-driven proton acceleration exhibited by measured laser absorptivity and reflectivity

    NASA Astrophysics Data System (ADS)

    Bin, J. H.; Allinger, K.; Khrennikov, K.; Karsch, S.; Bolton, P. R.; Schreiber, J.

    2017-03-01

    Proton acceleration from nanometer thin foils with intense laser pulses is investigated experimentally. We analyzed the laser absorptivity by parallel monitoring of laser transmissivity and reflectivity with different laser intensities when moving the targets along the laser axis. A direct correlation between laser absorptivity and maximum proton energy is observed. Experimental results are interpreted in analytical estimation, exhibiting a coexistence of plasma expansion and light-sail form of radiation pressure acceleration (RPA-LS) mechanisms during the entire proton acceleration process based on the measured laser absorptivity and reflectivity.

  1. Correction of optical absorption and scattering variations in laser speckle rheology measurements

    PubMed Central

    Hajjarian, Zeinab; Nadkarni, Seemantini K.

    2014-01-01

    Laser Speckle Rheology (LSR) is an optical technique to evaluate the viscoelastic properties by analyzing the temporal fluctuations of backscattered speckle patterns. Variations of optical absorption and reduced scattering coefficients further modulate speckle fluctuations, posing a critical challenge for quantitative evaluation of viscoelasticity. We compare and contrast two different approaches applicable for correcting and isolating the collective influence of absorption and scattering, to accurately measure mechanical properties. Our results indicate that the numerical approach of Monte-Carlo ray tracing (MCRT) reliably compensates for any arbitrary optical variations. When scattering dominates absorption, yet absorption is non-negligible, diffusing wave spectroscopy (DWS) formalisms perform similar to MCRT, superseding other analytical compensation approaches such as Telegrapher equation. The computational convenience of DWS greatly simplifies the extraction of viscoelastic properties from LSR measurements in a number of chemical, industrial, and biomedical applications. PMID:24663983

  2. Correction of optical absorption and scattering variations in Laser Speckle Rheology measurements.

    PubMed

    Hajjarian, Zeinab; Nadkarni, Seemantini K

    2014-03-24

    Laser Speckle Rheology (LSR) is an optical technique to evaluate the viscoelastic properties by analyzing the temporal fluctuations of backscattered speckle patterns. Variations of optical absorption and reduced scattering coefficients further modulate speckle fluctuations, posing a critical challenge for quantitative evaluation of viscoelasticity. We compare and contrast two different approaches applicable for correcting and isolating the collective influence of absorption and scattering, to accurately measure mechanical properties. Our results indicate that the numerical approach of Monte-Carlo ray tracing (MCRT) reliably compensates for any arbitrary optical variations. When scattering dominates absorption, yet absorption is non-negligible, diffusing wave spectroscopy (DWS) formalisms perform similar to MCRT, superseding other analytical compensation approaches such as Telegrapher equation. The computational convenience of DWS greatly simplifies the extraction of viscoelastic properties from LSR measurements in a number of chemical, industrial, and biomedical applications.

  3. Optoacoustic measurements of water vapor absorption at selected CO laser wavelengths in the 5-micron region

    NASA Technical Reports Server (NTRS)

    Menzies, R. T.; Shumate, M. S.

    1976-01-01

    Measurements of water vapor absorption were taken with a resonant optoacoustical detector (cylindrical pyrex detector, two BaF2 windows fitted into end plates at slight tilt to suppress Fabry-Perot resonances), for lack of confidence in existing spectral tabular data for the 5-7 micron region, as line shapes in the wing regions of water vapor lines are difficult to characterize. The measurements are required for air pollution studies using a CO laser, to find the differential absorption at the wavelengths in question due to atmospheric constituents other than water vapor. The design and performance of the optoacoustical detector are presented. Effects of absorption by ambient NO are considered, and the fixed-frequency discretely tunable CO laser is found suitable for monitoring urban NO concentrations in a fairly dry climate, using the water vapor absorption data obtained in the study.

  4. Working towards accreditation by the International Standards Organization 15189 Standard: how to validate an in-house developed method an example of lead determination in whole blood by electrothermal atomic absorption spectrometry.

    PubMed

    Garcia Hejl, Carine; Ramirez, Jose Manuel; Vest, Philippe; Chianea, Denis; Renard, Christophe

    2014-09-01

    Laboratories working towards accreditation by the International Standards Organization (ISO) 15189 standard are required to demonstrate the validity of their analytical methods. The different guidelines set by various accreditation organizations make it difficult to provide objective evidence that an in-house method is fit for the intended purpose. Besides, the required performance characteristics tests and acceptance criteria are not always detailed. The laboratory must choose the most suitable validation protocol and set the acceptance criteria. Therefore, we propose a validation protocol to evaluate the performance of an in-house method. As an example, we validated the process for the detection and quantification of lead in whole blood by electrothermal absorption spectrometry. The fundamental parameters tested were, selectivity, calibration model, precision, accuracy (and uncertainty of measurement), contamination, stability of the sample, reference interval, and analytical interference. We have developed a protocol that has been applied successfully to quantify lead in whole blood by electrothermal atomic absorption spectrometry (ETAAS). In particular, our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics.

  5. Determination of boron in blood, urine and bone by electrothermal atomic absorption spectrometry using zirconium and citric acid as modifiers

    NASA Astrophysics Data System (ADS)

    Burguera, Marcela; Burguera, José Luis; Rondón, Carlos; Carrero, Pablo

    2001-10-01

    A comparative study of various potential chemical modifiers (Au, Ba, Be, Ca, Cr, Ir, La, Lu, Mg, Ni, Pd, Pt, Rh, Ru, Sr, V, W, and Zr), and different 'coating' treatments (Zr, W, and W+Rh) of the pyrolytic graphite platform of a longitudinally heated graphite tube atomizer for thermal stabilization and determination of boron was undertaken. The use of Au, Ba, Be, Cr, Ir, Pt, Rh, Ru, Sr and V as modifiers, and of W+Rh coating produced erratic, and noisy signals, while the addition of La, Ni and Pd as modifiers, and the W coating had positive effects, but with too high background absorption signals, rendering their use unsuitable for boron determination even in aqueous solutions. The atomic absorption signal for boron was increased and stabilized when the platform was coated with Zr, and by the addition of Ca, Mg, Lu, W or Zr as modifiers. Only the addition of 10 μg of Zr as a modifier onto Zr-treated platforms allowed the use of a higher pyrolysis temperature without analyte losses. The memory effect was minimized by incorporating a cleaning step with 10 μl of 50 g l -1 NH 4F HF after every three boron measurements. The addition of 10 μl of 15 g l -1 citric acid together with Zr onto Zr-treated platforms significantly improved the characteristic mass to m0=282 pg, which is adequate for biological samples such as urine and bone, although the sensitivity was still inadequate for the determination of boron in blood of subjects without supplementary diet. Under optimized conditions, the detection limit (3σ) was 60 μg l -1. The amount of boron found in whole blood, urine and femur head samples from patients with osteoporosis was in agreement with values previously reported in the literature.

  6. Measurements of Cs absorption and retention in man

    SciTech Connect

    Henrichs, H.; Paretzke, H.G.; Voigt, G.; Berg, D. )

    1989-10-01

    One of the consequences of the Chernobyl reactor accident in 1986 was a comparatively high contamination of foodstuffs in Southern Federal Republic of Germany. In order to test radioecological models predicting the radiological consequences of such accidents, several thousand measurements were performed to determine Cs body burdens in members of the public. For the interpretation of these data and as a contribution to the improvement of the available database on the biokinetics of Cs isotopes in humans, we followed a small group of volunteers after their consumption of highly contaminated venison. Intakes, excretion rates and total body activities were measured during a period of more than 200 d. The data obtained were evaluated in terms of a compartment model to derive gastrointestinal uptakes, biological half-lives and dose conversion factors. The resulting uptake factors range from 65-90%, the half-lives of the long-term retention from 45 to 200 d. The majority of the resulting dose conversion factors lie below the values recommended by the ICRP, showing that the ICRP model is a reasonable and safe description of the Cs biokinetics in our study group, while the great variability of the results shows that it is not an accurate representation of the individual Cs retention.

  7. Determination of cadmium and lead at low levels by using preconcentration at fullerene coupled to thermospray flame furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Pereira, M. G.; Pereira-Filho, E. R.; Berndt, H.; Arruda, M. A. Z.

    2004-04-01

    A new and sensitive method for Cd and Pb determinations, based on the coupling of thermospray flame furnace atomic absorption spectrometry and a preconcentrator system, was developed. The procedure comprised the chelating of Cd and Pb with ammonium pyrrolidinedithiocarbamate with posterior adsorption of the chelates on a mixture (40 mg) of C 60 and C 70 at a flow rate of 2.0 ml min -1. These chelates were eluted from the adsorbent by passing a continuous flow of ethanol (80% v/v) at 0.9 ml min -1 to a nickel tube placed in an air/acetylene flame. After sample introduction into the tube by using a ceramic capillary (0.5 mm i.d.), the analytical signals were registered as peak height. Under these conditions, improvement factors in detectability of 675 and 200 were obtained for Cd and Pb, respectively, when compared to conventional flame atomic absorption spectrometry. Spiked samples (mineral and tap waters) and drinking water containing natural concentrations of Cd were employed for evaluating accuracy by comparing the results obtained from the proposed methodology with those using electrothermal atomic absorption spectrometry. In addition, certified reference materials (rye grass, CRM 281 and pig kidney, CRM 186) were also adopted for the accuracy tests. Due to the good linearity ranges for Cd (0.5-5.0 μg l -1) and Pb (10-250 μg l -1), samples with different concentrations could be analyzed. Detection limits of 0.1 and 2.4 μg l -1 were obtained for Cd and Pb, respectively, and RSD values <4.5% were observed ( n=10). Finally, a sample throughput of 24 determinations per hour was possible.

  8. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    NASA Astrophysics Data System (ADS)

    Grijalba, Alexander Castro; Martinis, Estefanía M.; Lascalea, Gustavo E.; Wuilloud, Rodolfo G.

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L- 1 and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L- 1 of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea.

  9. Multiple response optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry with sample injection as detergent emulsion

    NASA Astrophysics Data System (ADS)

    Brum, Daniel M.; Lima, Claudio F.; Robaina, Nicolle F.; Fonseca, Teresa Cristina O.; Cassella, Ricardo J.

    2011-05-01

    The present paper reports the optimization for Cu, Fe and Pb determination in naphtha by graphite furnace atomic absorption spectrometry (GF AAS) employing a strategy based on the injection of the samples as detergent emulsions. The method was optimized in relation to the experimental conditions for the emulsion formation and taking into account that the three analytes (Cu, Fe and Pb) should be measured in the same emulsion. The optimization was performed in a multivariate way by employing a three-variable Doehlert design and a multiple response strategy. For this purpose, the individual responses of the three analytes were combined, yielding a global response that was employed as a dependent variable. The three factors related to the optimization process were: the concentration of HNO 3, the concentration of the emulsifier agent (Triton X-100 or Triton X-114) in aqueous solution used to emulsify the sample and the volume of solution. At optimum conditions, it was possible to obtain satisfactory results with an emulsion formed by mixing 4 mL of the samples with 1 mL of a 4.7% w/v Triton X-100 solution prepared in 10% v/v HNO 3 medium. The resulting emulsion was stable for 250 min, at least, and provided enough sensitivity to determine the three analytes in the five samples tested. A recovery test was performed to evaluate the accuracy of the optimized procedure and recovery rates, in the range of 88-105%; 94-118% and 95-120%, were verified for Cu, Fe and Pb, respectively.

  10. A new supramolecular based liquid solid microextraction method for preconcentration and determination of trace bismuth in human blood serum and hair samples by electrothermal atomic absorption spectrometry.

    PubMed

    Kahe, Hadi; Chamsaz, Mahmoud

    2016-11-01

    A simple and reliable supramolecule-aggregated liquid solid microextraction method is described for preconcentration and determination of trace amounts of bismuth in water as well as human blood serum and hair samples. Catanionic microstructures of cetyltrimethylammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) surfactants, dissolved in deionized water/propanol, are used as a green solvent to extract bismuth (III)-diethyldithiocarbamate complexes by dispersive microextraction methodology. The extracted solid phase is easily removed and dissolved in 50 μL propanol for subsequent measurement by electrothermal atomic absorption spectrometry (ET-AAS). The procedure benefits the merits of supramolecule aggregates' properties and dispersive microextraction technique using water as the main component of disperser solvent, leading to direct interaction with analyte. Phase separation behavior of extraction solvent and different parameters influencing the extraction efficiency of bismuth ion such as salt concentration, pH, centrifugation time, amount of chelating agent, SDS:CTAB mole ratio, and solvent amounts were thoroughly optimized. Under the optimal experimental conditions, the calibration curve was linear in the range of 0.3-6 μg L(-1) Bi (III) with a limit of detection (LOD) of 0.16 μg L(-1) (S/N = 3). The relative standard deviations (RSD) of determination were obtained to be 5.1 and 6.2 % for 1 and 3 μg L(-1) of Bi (III), respectively. The developed method was successfully applied as a sensitive and accurate technique for determination of bismuth ion in human blood serum, hair samples, and a certified reference material.

  11. Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

    PubMed

    Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

    2015-01-01

    A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

  12. In situ emulsification microextraction using a dicationic ionic liquid followed by magnetic assisted physisorption for determination of lead prior to micro-sampling flame atomic absorption spectrometry.

    PubMed

    Shokri, Masood; Beiraghi, Asadollah; Seidi, Shahram

    2015-08-19

    For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L(-1) lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf2], was added into the sample solution containing 100 μL of 1.0 mol L(-1) 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl2, to form a water immiscible ionic liquid, [pbmim][NTf2]2. This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe3O4 magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf2]2, physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L(-1). Good linearity was obtained in the range of 2.5-150 μg L(-1) with determination coefficient (r(2)) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L(-1) was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples.

  13. On the possibilities of high-resolution continuum source graphite furnace atomic absorption spectrometry for the simultaneous or sequential monitoring of multiple atomic lines

    NASA Astrophysics Data System (ADS)

    Resano, M.; Rello, L.; Flórez, M.; Belarra, M. A.

    2011-05-01

    This paper explores the potential of commercially available high-resolution continuum source graphite furnace atomic absorption spectrometry instrumentation for the simultaneous or sequential monitoring of various atomic lines, in an attempt to highlight the analytical advantages that can be derived from this strategy. In particular, it is demonstrated how i) the monitoring of multiplets may allow for the simple expansion of the linear range, as shown for the measurement of Ni using the triplet located in the vicinity of 234.6 nm; ii) the use of a suitable internal standard may permit improving the precision and help in correcting for matrix-effects, as proved for the monitoring of Ni in different biological samples; iii) direct and multi-element analysis of solid samples may be feasible on some occasions, either by monitoring various atomic lines that are sufficiently close (truly simultaneous monitoring, as demonstrated in the determination of Co, Fe and Ni in NIST 1566a Oyster tissue) or, alternatively, by opting for a selective and sequential atomization of the elements of interest during every single replicate. Determination of Cd and Ni in BCR 679 White cabbage is attempted using both approaches, which permits confirming that both methods can offer very similar and satisfactory results. However, it is important to stress that the second approach provides more flexibility, since analysis is no longer limited to those elements that show very close atomic lines (closer than 0.3 nm in the ultraviolet region) with a sensitivity ratio similar to the concentration ratio of the analytes in the samples investigated.

  14. A study of the distribution of aluminum in human placental tissues based on alkaline solubilization with determination by electrothermal atomic absorption spectrometry

    PubMed Central

    Kruger, Pamela C.; Schell, Lawrence M.; Stark, Alice D.; Parsons, Patrick J.

    2010-01-01

    Summary Aluminum (Al) is a nonessential element known to induce neurotoxic effects, such as dialysis dementia, in patients on hemodialysis, with compromised kidney function. The role of Al in the progression of some neurodegenerative diseases, such as Alzheimer’s disease (AD), is controversial, and remains unclear. The effects of Al on other vulnerable populations, such as fetuses and infants, have been infrequently studied. In the present study, Al has been measured in human placenta samples, comprising ~160 each of placenta bodies, placenta membranes, and umbilical cords, using electrothermal atomic absorption spectrometry (ETAAS) after atmospheric pressure digestion with tetramethylammonium hydroxide (TMAH) and ethylenediaminetetraacidic acid (EDTA). The sensitivity, or characteristic mass (m0), for Al at the 309.3-nm line was found to be 30 ± 4 pg. The instrumental detection limit (IDL) (3s) for Al in solution was calculated as 0.72 μg L-1, while the method detection limit (MDL) (3s) was 0.25 μg g-1. Accuracy was assessed through analysis of quality control (QC) materials, including certified reference materials (CRMs), in-house reference materials (RMs), and spike recovery experiments, of varying matrices. Placental tissue analyses revealed geometric mean concentrations of approximately 0.5 μg g-1 Al in placenta bodies (n=165) and membranes (n=155), while Al concentrations in the umbilical cord (n=154) were about 0.3 μg g-1. Al was detected in 95% of placenta bodies, and 81% of placenta membranes, but only in 46% of umbilical cords. PMID:21072353

  15. Determination of antimony, arsenic, bismuth, selenium, tellurium and tin by low pressure atomic absorption spectrometry with a quartz tube furnace atomizer and hydride generation with air addition.

    PubMed

    Zhang, B; Wang, Y; Wang, X; Chen, X; Feng, J

    1995-08-01

    A new method has been developed for the determination of antimony, arsenic, bismuth, selenium, tellurium and tin by hydride generation-atomic absorption spectrometry in an electrically heated quartz tube furnace under sub-atmospheric pressure. The hydride generator, operating at a pressure lower than atmospheric, is used to generate and collect the hydrides of these elements. A certain volume (at atmospheric pressure) of air is then added to the generator after the formation of the volatile hydride. The gaseous mixture of the hydride and air is drawn into an evacuated, heated quartz tube by a vacuum pump. The proposed method gives improved sensitivities and detection limits.

  16. [Determination of Pb and Cd in atomospheric particulates by flame atomic absorption spectrometry coupled with on-line flow injection pretreatment with ultrasonic leaching].

    PubMed

    Gao, Yan; Wang, Dong-hai; Lin, Yu-bin; Li, Jian-yi; Kong, Qing-zhen

    2003-04-01

    In this paper, the method for extracting the metals from the filter membrane of the atomospheric particulates with ultrasonic leaching was reported. The dissolution conditions of kinds and acidity as well as the interference conditions were studied. The method of determination Pb and Cd of the atomospheric particulates by flame atomic absorption spectrometry coupled with on-line flow injection preconcentration was proved to be rapid and accuracy. The recoveries are more than 97%. The relative standard deviation of six samples are less than 2.6%.

  17. Mesoporous Silica Nanoparticles as an Adsorbent for Preconcentration and Determination of Trace Amount of Nickel in Environmental Samples by Atom Trap Flame Atomic Absorption Spectrometry

    NASA Astrophysics Data System (ADS)

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

    2016-01-01

    A rapid enrichment method based on solid-phase extraction (SPE) has been established for preconcentration and separation of trace Ni(II) ions in water samples prior to their determination by atom trap flame atomic absorption spectrometry. A column filled with bulky NH2-UVM7 was used as the novel adsorbent. Under optimal conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were 3-92 μg/L, 0.8 μg/L, and 100, respectively. The validity of the method was checked by the standard reference material.

  18. Effect of Water Vapor Absorption on Measurements of Atmospheric Nitrate Radical by LP-DOAS

    NASA Astrophysics Data System (ADS)

    Li, Su-wen; Liu, Wen-qing; Xie, Pin-hua; Yang, Yi-jun; Chen, De-bao; Li, Zheng

    2008-10-01

    During the measurement of atmospheric nitrate radical by long-path differential optical absorption spec-troscopy, water vapor strong absorption could affect the measurement of nitrate radical and detection limits of system. Under the tropospheric condition, the optical density of water vapor absorption is non-linearly dependent on column density. An effective method was developed to eliminate the effect of water vapor absorption. Reference spectra of water vapor based on the daytime atmospheric absorption spectra, when fitted together with change of cross section with water vapor column densities, gave a more accurate fitting of water vapor absorptions, thus its effect on the measurements of nitrate radical could be restricted to a minimum and detection limits of system reached 3.6 ppt. The modified method was applied during an intensive field campaign in the Pearl River Delta, China. The NO3 concentration in polluted air masses varied from 3.6 ppt to 82.5 ppt with an average level of 23.6±1.8 ppt.

  19. [Development of a photoacoustic spectroscopy system for the measurement of absorption coefficient of atmospheric aerosols].

    PubMed

    Liu, Qiang; Niu, Ming-Sheng; Wang, Gui-Shi; Cao, Zhen-Song; Liu, Kun; Chen, Wei-Dong; Gao, Xiao-Ming

    2013-07-01

    In the present paper, the authors focus on the effect of the resonance frequency shift due to the changes in temperature and humidity on the PA signal, present several methods to control the noise derived form gas flow and vibration from the sampling pump. Based on the efforts mentioned above, a detection limit of 1.4 x 10(-8) W x cm(-1) x Hz(-1/2) was achieved for the measurement of atmospheric aerosols absorption coefficient. During the experiments, the PA cell was calibrated with the absorption of standard NO2 gas at 532 nm and the atmospheric aerosols were measured continuously. The measurement results show that the PAS is suitable for the real-time measurement of the absorption coefficient of atmospheric aerosols in their natural suspended state.

  20. Vacuum Ultraviolet Absorption Measurements of Atomic Oxygen in a Shock Tube

    NASA Technical Reports Server (NTRS)

    Meyer, Scott Andrew

    1995-01-01

    The absorption of vacuum ultraviolet light by atomic oxygen has been measured in the Electric Arc-driven Shock Tube (EAST) Facility at NASA-Ames Research Center. This investigation demonstrates the instrumentation required to determine atomic oxygen concentrations from absorption measurements in impulse facilities. A shock wave dissociates molecular oxygen, producing a high temperature sample of atomic oxygen in the shock tube. A probe beam is generated with a Raman-shifted ArF excimer laser. By suitable tuning of the laser, absorption is measured over a range of wavelengths in the region of the atomic line at 130.49 nm. The line shape function is determined from measurements at atomic oxygen densities of 3x10(exp 17) and 9x10(exp 17) cm(exp -3). The broadening coefficient for resonance interactions is deduced from this data, and this value is in accord with available theoretical models.

  1. Vacuum Ultraviolet Absorption Measurements of Atomic Oxygen in a Shock Tube

    NASA Technical Reports Server (NTRS)

    Meyer, Scott Andrew

    1995-01-01

    The absorption of vacuum ultraviolet light by atomic oxygen has been measured in the Electric Arc-driven Shock Tube (EAST) Facility at NASA-Ames Research Center. This investigation demonstrates the instrumentation required to determine atomic oxygen concentrations from absorption measurements in impulse facilities. A shock wave dissociates molecular oxygen, producing a high temperature sample of atomic oxygen in the shock tube. A probe beam is generated with a Raman-shifted ArF excimer laser. By suitable tuning of the laser, absorption is measured over a range of wavelengths in the region of the atomic line at 130.49 nm. The line shape function is determined from measurements at atomic oxygen densities of 3 x 10(exp 17) and 9 x 10(exp 17) cm(exp -3). The broadening coefficient for resonance interactions is deduced from this data, and this value is in accord with available theoretical models.

  2. Vacuum Ultraviolet Absorption Measurements of Atomic Oxygen in a Shock Tube

    NASA Technical Reports Server (NTRS)

    Meyer, Scott Andrew

    1995-01-01

    The absorption of vacuum ultraviolet light by atomic oxygen has been measured in the Electric Arc-driven Shock Tube (EAST) Facility at NASA-Ames Research Center. This investigation demonstrates the instrumentation required to determine atomic oxygen concentrations from absorption measurements in impulse facilities. A shock wave dissociates molecular oxygen, producing a high temperature sample of atomic oxygen in the shock tube. A probe beam is generated with a Raman-shifted ArF excimer laser. By suitable tuning of the laser, absorption is measured over a range of wavelengths in the region of the atomic line at 130.49 nm. The line shape function is determined from measurements at atomic oxygen densities of 3 x 10(exp 17) and 9 x 10(exp 17)/cu cm. The broadening coefficient for resonance interactions is deduced from this data, and this value is in accord with available theoretical models.

  3. Measurement of Hydrogen Chloride in Coal-Fired Power Plant Emissions Using Tunable Diode Laser Spectrometry

    NASA Astrophysics Data System (ADS)

    Mackay, K. L.; Chanda, A.; Mackay, G.; Pisano, J. T.; Durbin, T. D.; Crabbe, K.; Smith, T.

    2016-09-01

    In this paper, we report on TDL HCl measurements obtained at a coal-fi red power plant which indicate that there is a significant perturbation of the HCl absorption feature. A methodology was also developed to remediate this effect and provide accurate measurement that will meet the EPA precision and detection limits currently being developed for HCl measurements of process gas emissions.

  4. Galileo infrared imaging spectrometry measurements at the Moon

    NASA Astrophysics Data System (ADS)

    McCord, T. B.; Soderblom, L. A.; Carlson, R. W.; Fanale, F. P.; Lopes-Gautier, R.; Ocampo, A. C.; Forsythe, J.; Campell, B.; Granahan, J. C.; Smythe, W. D.; Weissmann, P. R.; Becker, K. J.; Edwards, K.; Kamp, L.; Lo, J.; Mehlman, R.; Torson, J.; Danielson, G. E.; Matson, D. L.; Kieffer, H. H.; Johnson, T. V.

    1994-03-01

    Imaging spectrometer observations were made of the surface of the Moon during the December 1990 flyby of the Earth-Moon system by the Galileo spacecraft. This article documents this data set and presents analyses of some of the data. The near infrared mapping spectrometer (NIMS) investigation obtained 17 separate mosaics of the Moon in 408 spectral channels between about 0.7 and 5.2 micrometers. The instrument was originally designed to operate in orbit about Jupiter and therefore saturates at many spectral channels for most measurement situations at 1 AU. However, sufficient measurements were made of the Moon to verify the proper operation of the instrument and to demonstrate its capabilities. Analysis of these data show that the NIMS worked as expected and produced measurements consistent with previous ground-based telescopic studies. These are the first imaging spectrometer measurements of this type from space for the Moon, and they illustrate several major points concerning this type of observation and about the NIMS capabilities specifically. Of major importance are the difference between framing and scanning instruments and the effects of the spacecraft and the scan platform on the performance of such and experiment. The science return of subsequent NIMS and other investigation measurements will be significantly enhanced by the experience and results gained.

  5. Galileo infrared imaging spectrometry measurements at the Moon

    NASA Technical Reports Server (NTRS)

    Mccord, Thomas B.; Soderblom, Larry A.; Carlson, Robert W.; Fanale, Fraser P.; Lopes-Gautier, Rosaly; Ocampo, Adriano; Forsythe, Jennifer; Campbell, Bruce; Granahan, James C.; Smythe, W. D.

    1994-01-01

    Imaging spectrometer observations were made of the surface of the Moon during the December 1990 flyby of the Earth-Moon system by the Galileo spacecraft. This article documents this data set and presents analyses of some of the data. The near infrared mapping spectrometer (NIMS) investigation obtained 17 separate mosaics of the Moon in 408 spectral channels between about 0.7 and 5.2 micrometers. The instrument was originally designed to operate in orbit about Jupiter and therefore saturates at many spectral channels for most measurement situations at 1 AU. However, sufficient measurements were made of the Moon to verify the proper operation of the instrument and to demonstrate its capabilities. Analysis of these data show that the NIMS worked as expected and produced measurements consistent with previous ground-based telescopic studies. These are the first imaging spectrometer measurements of this type from space for the Moon, and they illustrate several major points concerning this type of observation and about the NIMS capabilities specifically. Of major importance are the difference between framing and scanning instruments and the effects of the spacecraft and the scan platform on the performance of such and experiment. The science return of subsequent NIMS and other investigation measurements will be significantly enhanced by the experience and results gained.

  6. Photothermal self-phase-modulation technique for absorption measurements on high-reflective coatings.

    PubMed

    Steinlechner, Jessica; Jensen, Lars; Krüger, Christoph; Lastzka, Nico; Steinlechner, Sebastian; Schnabel, Roman

    2012-03-10

    We propose and demonstrate a new measurement technique for the optical absorption of high-reflection coatings. Our technique is based on photothermal self-phase modulation and exploits the deformation of cavity Airy peaks that occurs due to coating absorption of intracavity light. The mirror whose coating is under investigation needs to be the input mirror of a high-finesse cavity. Our example measurements were performed on a high-reflection SiO2-Ta2O5 coating in a three-mirror ring-cavity setup at a wavelength of 1064 nm. The optical absorption of the coating was determined to be α=(23.9±2.0)·10(-6) per coating. Our result is in excellent agreement with an independently performed laser calorimetry measurement that gave a value of α=(24.4±3.2)·10(-6) per coating. Since the self-phase modulation in our coating-absorption measurement affects mainly the propagation through the cavity input mirror, our measurement result is practically uninfluenced by the optical absorption of the other cavity mirrors.

  7. Simultaneous bidirectional magnesium ion flux measurements in single barnacle muscle cells by mass spectrometry

    SciTech Connect

    Montes, J.G.; Sjodin, R.A.; Yergey, A.L.; Vieira, N.E. )

    1989-09-01

    Stable isotopes of Mg were used to measure bidirectional magnesium ion fluxes in single barnacle giant muscle fibers immersed in Ca- and Na-free, isosmotic media. Measurements were made using a mass spectrometric technique, thermal ionization mass spectrometry (TIMS), in conjunction with atomic absorption spectroscopy. Kinetic relations based on a first-order model were developed that permit the determination of unidirectional rate coefficients for Mg influx, ki, and efflux, ke, in the same experiment from knowledge of initial conditions and the initial and final ratios of 26Mg/24Mg and 25Mg/24Mg in ambient solutions (i.e., by isotope dilution). Such determinations were made for three values of the external Mg ion concentration: 5, 25, and 60 mM. At the concentration (Mg+2)o = 5 mM, ki and ke were about equal at a value of 0.01 min-1. At the higher values of (Mg+2)o, the values of ke increased along a curve suggesting saturation, whereas the values of ki remained essentially constant. As could be expected on the basis of a constant ki, the initial influx rate varied in direct linear proportion to (Mg+2)o, and was 11.8 pmol/cm2s when (Mg+2)o was 5 mM. However, the initial efflux rate appeared to increase nonlinearly with (Mg+2)o, varying from 13.4 pmol/cm2s (( Mg+2)o = 5 mM) to approximately 80 pmol/cm2s ((Mg+2)o = 60 mM). The results are consistent with a model that assumes Mg influx to be mainly an electrodiffusive inward leak with PMg = 0.07 cm/s and Mg efflux to be almost entirely by active transport processes. Where comparisons can be made, the rate coefficients determined from stable isotope measurements agree with those previously obtained using radioactive Mg. The rate coefficients can be used to correctly predict time-dependent changes in total fiber Mg content.

  8. A 2-Micron Pulsed Integrated Path Differential Absorption Lidar Development For Atmospheric CO2 Concentration Measurements

    NASA Technical Reports Server (NTRS)

    Yu, Jirong; Petros, Mulugeta; Reithmaier, Karl; Bai, Yingxin; Trieu, Bo C.; Refaat, Tamer F.; Kavaya, Michael J.; Singh, Upendra N.

    2012-01-01

    A 2-micron pulsed, Integrated Path Differential Absorption (IPDA) lidar instrument for ground and airborne atmospheric CO2 concentration measurements via direct detection method is being developed at NASA Langley Research Center. This instrument will provide an alternate approach to measure atmospheric CO2 concentrations with significant advantages. A high energy pulsed approach provides high-precision measurement capability by having high signal-to-noise level and unambiguously eliminates the contamination from aerosols and clouds that can bias the IPDA measurement.

  9. [Research on the NO2 mean concentration measurement with target differential optical absorption spectroscopy technology].

    PubMed

    Liu, Jin; Si, Fu-Qi; Zhou, Hai-Jin; Zhao, Min-Jie; Dou, Ke; Liu, Wen-Qing

    2013-04-01

    A new monitoring method of NO2 concentration near ground with the target difference absorption spectrum technology (Target DOAS) is introduced in the present paper. This method is based on the passive difference absorption spectrum technology. The instrument collects solar reflection spectrum of remote objectives, such as wall of building and mountain, and a specific reference spectrum is chosen to subtract the influence of trace gases from the target to atmospheric top, then integrated concentration of NO2 along the path between the target and instrument can be calculated through the differential absorption spectra inversion algorithm. Since the distance between the instrument and target is given, the mean concentration of NO2 can be derived. With developed Target DOAS instrument, NO2 concentration measurement was carried out in Hefei. And comparison was made between the target DOAS and long path difference absorption spectrometer. Good consistency was presented, proving the feasibility of this method.

  10. Quantitative photoacoustic measurement of tissue optical absorption spectrum aided by an optical contrast agent.

    PubMed

    Rajian, Justin Rajesh; Carson, Paul L; Wang, Xueding

    2009-03-16

    In photoacoustic imaging, the intensity of photoacoustic signal induced by optical absorption in biological tissue is proportional to light energy deposition, which is the product of the absorption coefficient and the local light fluence. Because tissue optical properties are highly dependent on the wavelength, the spectrum of the local light fluence at a target tissue beneath the sample surface is different than the spectrum of the incident light fluence. Therefore, quantifying the tissue optical absorption spectrum by using a photoacoustic technique is not feasible without the knowledge of the local light fluence. In this work, a highly accurate photoacoustic measurement of the subsurface tissue optical absorption spectrum has been achieved for the first time by introducing an extrinsic optical contrast agent with known optical properties. From the photoacoustic measurements with and without the contrast agent, a quantified measurement of the chromophore absorption spectrum can be realized in a strongly scattering medium. Experiments on micro-flow vessels containing fresh canine blood buried in phantoms and chicken breast tissues were carried out in a wavelength range from 680 nm to 950 nm. Spectroscopic photoacoustic measurements of both oxygenated and deoxygenated blood specimens presented an improved match with the references when employing this technique.

  11. Servo-amplifiers for ion current measurement in mass spectrometry

    USGS Publications Warehouse

    Stacey, J.S.; Russell, R.D.; Kollar, F.

    1965-01-01

    A servo-voltmeter can provide a useful alternative to the d.c. amplifier or vibrating reed electrometer for the accurate measurement of mass spectrometer ion currents, and has some advantages which recommend its use in certain applications. A generalized analysis based on servomechanism theory is presented as an aid for understanding the design criteria for this type of device. Two existing systems are described and their operation and performance are examined.

  12. First neutron spectrometry measurement at the HL-2A Tokamak

    NASA Astrophysics Data System (ADS)

    Yuan, Xi; Zhang, Xing; Xie, Xu-Fei; Chen, Zhong-Jing; Peng, Xing-Yu; Fan, Tie-Shuan; Chen, Jin-Xiang; Li, Xiang-Qing; Yuan, Guo-Liang; Yang, Qing-Wei; Yang, Jin-Wei

    2013-12-01

    A compact neutron spectrometer based on the liquid scintillator is presented for neutron energy spectrum measurements at the HL-2A Tokamak. The spectrometer was well characterized and a fast digital pulse shape discrimination software was developed using the charge comparison method. A digitizer data acquisition system with a maximum frequency of 1 MHz can work under an environment with a high count rate at HL-2A Tokamak. Specific radiation and magnetic shielding for the spectrometer were designed for the neutron spectrum measurement at the HL-2A Tokamak. For pulse height spectrum analysis, dedicated numerical simulation utilizing NUBEAM combined with GENESIS was performed to obtain the neutron energy spectrum. Subsequently, the transportation process from the plasma to the detector was evaluated with Monte Carlo calculations. The distorted neutron energy spectrum was folded with the response matrix of the liquid scintillation spectrometer, and good consistency was found between the simulated and measured pulse height spectra. This neutron spectrometer based on a digital acquisition system could be well adopted for the investigation of the auxiliary heating behavior and the fast-ion related phenomenon on different tokamak devices.

  13. Photo-acoustic measurements of gas and aerosol absorption with diode lasers.

    PubMed

    Ponomarev, Yu N

    2004-12-01

    The results of designing multipurpose high-sensitive photo-acoustic (PA) detectors and their application to high-resolution diode laser spectroscopy of molecular gases, gas analysis, and aerosol absorption measurements are summarized in this paper. The hardware and software of the diode laser spectrometer with a Helmholtz resonant PA detector providing an absorption sensitivity limit of better than 10(-7)Wm(-1)Hz(-1/2) are described. A procedure is proposed for an experiment involving the measurements of the rotational structure of hot vibrational bands of molecules. The results of the application of the nonresonant PA cell with temporal resolution of signals to measurements of weak nonresonant absorption of gases and soot aerosols are presented, and the possibility of creating a broad-band PA laser diode aerosol-meter is discussed.

  14. Measurement of transient gas flow parameters by diode laser absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Bolshov, M. A.; Kuritsyn, Yu A.; Liger, V. V.; Mironenko, V. R.; Nadezhdinskii, A. I.; Ponurovskii, Ya Ya; Leonov, S. B.; Yarantsev, D. A.

    2015-04-01

    An absorption spectrometer based on diode lasers is developed for measuring two-dimension maps of temperature and water vapour concentration distributions in the combustion zones of two mixing supersonic flows of fuel and oxidiser in the single run regime. The method of measuring parameters of hot combustion zones is based on detection of transient spectra of water vapour absorption. The design of the spectrometer considerably reduces the influence of water vapour absorption along the path of a sensing laser beam outside the burning chamber. The optical scheme is developed, capable of matching measurement results in different runs of mixture burning. A new algorithm is suggested for obtaining information about the mixture temperature by constructing the correlation functions of the experimental spectrum with those simulated from databases. A two-dimensional map of temperature distribution in a test chamber is obtained for the first time under the conditions of plasma-induced combusion of the ethylene - air mixture.

  15. Synchrotron Photoionization Mass Spectrometry Measurements of Kinetics and Product Formation in the Allyl Radical (H2CCHCH2)Self Reaction

    NASA Technical Reports Server (NTRS)

    Selby, Talitha M.; Melini, giovanni; Goulay, Fabien; Leone, Stephen R.; Fahr, Askar; Taatjes, Craig A.; Osborn, David L.

    2008-01-01

    Product channels for the self-reaction of the resonance-stabilized allyl radical, C3H5 + C3H5, have been studied with isomeric specificity at temperatures from 300-600 K and pressures from 1-6 Torr using time-resolved multiplexed photoionization mass spectrometry. Under these conditions 1,5-hexadiene was the only C6H10 product isomer detected. The lack of isomerization of the C6H10 product is in marked contrast to the C6H6 product in the related C3H3 + C3H3 reaction, and is due to the more saturated electronic structure of the C6H10 system. The disproportionation product channel, yielding allene + propene, was also detected, with an upper limit on the branching fraction relative to recombination of 0.03. Analysis of the allyl radical decay at 298 K yielded a total rate coefficient of (2.7 +/- 0.8) x 10(exp -11) cu cm/molecule/s, in good agreement with pre.vious experimental measurements using ultraviolet kinetic absorption spectroscopy and a recent theoretical determination using variable reaction coordinate transition state theory. This result provides independent indirect support for the literature value of the allyl radical ultraviolet absorption cross-section near 223 nm.

  16. Boron concentration measurement in biological tissues by charged particle spectrometry.

    PubMed

    Bortolussi, S; Altieri, S

    2013-11-01

    Measurement of boron concentration in biological tissues is a fundamental aspect of boron neutron capture therapy, because the outcome of the therapy depends on the distribution of boron at a cellular level, besides on its overall concentration. This work describes a measurement technique based on the spectroscopy of the charged particles emitted in the reaction (10)B(n,α)(7)Li induced by thermal neutrons, allowing for a quantitative determination of the boron concentration in the different components that may be simultaneously present in a tissue sample, such as healthy cells, tumor cells and necrotic cells. Thin sections of tissue containing (10)B are cut at low temperatures and irradiated under vacuum in a thermal neutron field. The charged particles arising from the sample during the irradiation are collected by a thin silicon detector, and their spectrum is used to determine boron concentration through relatively easy calculations. The advantages and disadvantages of this technique are here described, and validation of the method using tissue standards with known boron concentrations is presented.

  17. Evaluation of solid sampling for determination of Mo, Ni, Co, and V in soil by high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Babos, Diego Victor; Barros, Ariane Isis; Ferreira, Edilene Cristina; Neto, José Anchieta Gomes

    2017-04-01

    New methods are proposed for the determination of Mo, Ni, Co, and V in soils using high-resolution continuum source graphite furnace atomic absorption spectrometry with direct solid sampling. Cobalt and V were simultaneously determined, and different analytical lines of Ni and V were monitored to adjust sensitivity for each sample. Accuracy was checked by means of soil certified reference materials, and also by flame atomic absorption spectrometry as comparative technique. The results for Mo, Ni, Co, and V found by proposed methods were in agreement with certified values and with those obtained by the comparative technique at 95% confidence level. The concentrations found in different soil samples were in the ranges 0.19-1.84 mg kg- 1 (Mo), 9.2-22.7 mg kg- 1 (Ni), 1.1-10.7 mg kg- 1 (Co), and 35.6-426.1 mg kg- 1 (V). The relative standard deviations were in the ranges 3.2-10% (Mo), 2.8-9.8% (Ni), 4.0-9.2% (Co), and 1.2-8.0% (V). The limits of quantification for Mo, Ni, Co, and V were 0.027, 0.071, 0.15, and 1.43 ng, respectively.

  18. Application of dual-cloud point extraction for the trace levels of copper in serum of different viral hepatitis patients by flame atomic absorption spectrometry: A multivariate study

    NASA Astrophysics Data System (ADS)

    Arain, Salma Aslam; Kazi, Tasneem G.; Afridi, Hassan Imran; Abbasi, Abdul Rasool; Panhwar, Abdul Haleem; Naeemullah; Shanker, Bhawani; Arain, Mohammad Balal

    2014-12-01

    An efficient, innovative preconcentration method, dual-cloud point extraction (d-CPE) has been developed for the extraction and preconcentration of copper (Cu2+) in serum samples of different viral hepatitis patients prior to couple with flame atomic absorption spectrometry (FAAS). The d-CPE procedure was based on forming complexes of elemental ions with complexing reagent 1-(2-pyridylazo)-2-naphthol (PAN), and subsequent entrapping the complexes in nonionic surfactant (Triton X-114). Then the surfactant rich phase containing the metal complexes was treated with aqueous nitric acid solution, and metal ions were back extracted into the aqueous phase, as second cloud point extraction stage, and finally determined by flame atomic absorption spectrometry using conventional nebulization. The multivariate strategy was applied to estimate the optimum values of experimental variables for the recovery of Cu2+ using d-CPE. In optimum experimental conditions, the limit of detection and the enrichment factor were 0.046 μg L-1 and 78, respectively. The validity and accuracy of proposed method were checked by analysis of Cu2+ in certified sample of serum (CRM) by d-CPE and conventional CPE procedure on same CRM. The proposed method was successfully applied to the determination of Cu2+ in serum samples of different viral hepatitis patients and healthy controls.

  19. Application of dual-cloud point extraction for the trace levels of copper in serum of different viral hepatitis patients by flame atomic absorption spectrometry: a multivariate study.

    PubMed

    Arain, Salma Aslam; Kazi, Tasneem G; Afridi, Hassan Imran; Abbasi, Abdul Rasool; Panhwar, Abdul Haleem; Naeemullah; Shanker, Bhawani; Arain, Mohammad Balal

    2014-12-10

    An efficient, innovative preconcentration method, dual-cloud point extraction (d-CPE) has been developed for the extraction and preconcentration of copper (Cu(2+)) in serum samples of different viral hepatitis patients prior to couple with flame atomic absorption spectrometry (FAAS). The d-CPE procedure was based on forming complexes of elemental ions with complexing reagent 1-(2-pyridylazo)-2-naphthol (PAN), and subsequent entrapping the complexes in nonionic surfactant (Triton X-114). Then the surfactant rich phase containing the metal complexes was treated with aqueous nitric acid solution, and metal ions were back extracted into the aqueous phase, as second cloud point extraction stage, and finally determined by flame atomic absorption spectrometry using conventional nebulization. The multivariate strategy was applied to estimate the optimum values of experimental variables for the recovery of Cu(2+) using d-CPE. In optimum experimental conditions, the limit of detection and the enrichment factor were 0.046μgL(-1) and 78, respectively. The validity and accuracy of proposed method were checked by analysis of Cu(2+) in certified sample of serum (CRM) by d-CPE and conventional CPE procedure on same CRM. The proposed method was successfully applied to the determination of Cu(2+) in serum samples of different viral hepatitis patients and healthy controls.

  20. Investigating effects of sample pretreatment on protein stability using size-exclusion chromatography and high-resolution continuum source atomic absorption spectrometry.

    PubMed

    Rakow, Tobias; El Deeb, Sami; Hahne, Thomas; El-Hady, Deia Abd; AlBishri, Hassan M; Wätzig, Hermann

    2014-09-01

    In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%.

  1. Determination of lead in blood by chelation with ammonium pyrrolidine dithio-carbamate followed by tungsten-coil atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Salido, Arthur; Sanford, Caryn L.; Jones, Bradley T.

    1999-08-01

    An inexpensive, bench-top blood Pb analyzer has been developed. The system is based on tungsten-coil atomic absorption spectrometry. Pb atomization occurs on W-coils extracted from commercially available slide projector bulbs. The system has minimal power requirements: 120 ACV and 15 A. A small, computer-controlled CCD spectrometer is used as the detector. A Pb hollow cathode lamp is used as the source. Blood Pb is chelated with ammonium pyrrolidine dithio-carbamate and extracted into methyl iso-butyl ketone (4-methyl 2-pentanone). Twenty-microliter volumes of the organic phase are deposited on the W-coil, dried at 1.4 A, charred at 2.3 A and atomized at 6.0 A. Graphite furnace atomic absorption spectrometry is used as a comparison for W-coil results. Levels 1-4 of a NIST standard reference material 955b ‘lead in bovine blood’ are used to test accuracy and precision. The analytical figures of merit for the system are: 12-pg instrument detection limit, 24-pg blood detection limit and a characteristic mass of 28 pg.

  2. Pressure Measurements Using an Airborne Differential Absorption Lidar. Part 1; Analysis of the Systematic Error Sources

    NASA Technical Reports Server (NTRS)

    Flamant, Cyrille N.; Schwemmer, Geary K.; Korb, C. Laurence; Evans, Keith D.; Palm, Stephen P.

    1999-01-01

    Remote airborne measurements of the vertical and horizontal structure of the atmospheric pressure field in the lower troposphere are made with an oxygen differential absorption lidar (DIAL). A detailed analysis of this measurement technique is provided which includes corrections for imprecise knowledge of the detector background level, the oxygen absorption fine parameters, and variations in the laser output energy. In addition, we analyze other possible sources of systematic errors including spectral effects related to aerosol and molecular scattering interference by rotational Raman scattering and interference by isotopic oxygen fines.

  3. Cryogenic Thermal Absorptance Measurements on Small-Diameter Stainless Steel Tubing

    NASA Technical Reports Server (NTRS)

    Tuttle, James; Jahromi, Amir; Canavan, Edgar; DiPirro, Michael

    2015-01-01

    The Mid Infrared Instrument (MIRI) on the James Webb Space Telescope includes a mechanical cryocooler which cools its detectors to their 6 Kelvin operating temperature. The coolant gas flows through several meters of small-diameter stainless steel tubing, which is exposed to thermal radiation from its environment. Over much of its length this tubing is gold-plated to minimize the absorption of this radiant heat. In order to confirm that the cryocooler will meet MIRI's requirements, the thermal absorptance of this tubing was measured as a function of its environment temperature. We describe the measurement technique and present the results.

  4. A photophonic instrument concept to measure atmospheric aerosol absorption. M.S. Thesis

    NASA Technical Reports Server (NTRS)

    Engle, C. D.

    1982-01-01

    A laboratory model of an instrument to measure the absorption of atmospheric aerosols was designed, built, and tested. The design was based on the photophonic phenomenon discovered by Bell and an acoustic resonator developed by Helmholtz. Experiments were done to show ways the signal amplitude could be improved and the noise reduced and to confirm the instrument was sensitive enough to be practical. The research was undertaken to develop concepts which show promise of being improvements on the instruments that are presently used to measure the absorption of the Sun's radiation by the Earth's atmospheric aerosols.

  5. Intersubband infrared absorption in Ge(x)Si(1-x)/Si superlattice by photocurrent measurement

    NASA Technical Reports Server (NTRS)

    Karunasiri, R. P. G.; Park, J. S.; Wang, K. L.; Cheng, Li-Jen

    1990-01-01

    The intersubband IR absorption of holes in a Ge(x)Si(1-x)/Si superlattice is observed for the first time. In the experiment, the photocurrent is measured as a function of applied bias which is used to inject holes to the minibands of the superlattice. Two peaks in the photocurrent as a function of bias across the device are observed due to intersubband absorption between the ground to the first and the first of the second light hole minibands. The polarization dependence measurement is used to study the nature of the transitions and is in good agreement with the selection rules.

  6. Airborne differential absorption lidar system for measurements of atmospheric water vapor and aerosols.

    PubMed

    Higdon, N S; Browell, E V; Ponsardin, P; Grossmann, B E; Butler, C F; Chyba, T H; Mayo, M N; Allen, R J; Heuser, A W; Grant, W B; Ismail, S; Mayor, S D; Carter, A F

    1994-09-20

    An airborne differential absorption lidar (DIAL) system has been developed at the NASA Langley Research Center for remote measurements of atmospheric water vapor (H(2)O) and aerosols. A solid-state alexandrite laser with a 1-pm linewidth and > 99.85% spectral purity was used as the on-line transmitter. Solid-state avalanche photodiode detector technology has replaced photomultiplier tubes in the receiver system, providing an average increase by a factor of 1.5-2.5 in the signal-to-noise ratio of the H(2)O measurement. By incorporating advanced diagnostic and data-acquisition instrumentation into other subsystems, we achieved additional improvements in system operational reliability and measurement accuracy. Laboratory spectroscopic measurements of H(2)O absorption-line parameters were perfo med to reduce the uncertainties in our knowledge of the absorption cross sections. Line-center H(2)O absorption cross sections were determined, with errors of 3-6%, for more than 120 lines in the 720-nm region. Flight tests of the system were conducted during 1989-1991 on the NASA Wallops Flight Facility Electra aircraft, and extensive intercomparison measurements were performed with dew-point hygrometers and H(2)O radiosondes. The H(2)O distributions measured with the DIAL system differed by ≤ 10% from the profiles determined with the in situ probes in a variety of atmospheric conditions.

  7. Airborne differential absorption lidar system for measurements of atmospheric water vapor and aerosols

    NASA Technical Reports Server (NTRS)

    Carter, Arlen F.; Allen, Robert J.; Mayo, M. Neale; Butler, Carolyn F.; Grossman, Benoist E.; Ismail, Syed; Grant, William B.; Browell, Edward V.; Higdon, Noah S.; Mayor, Shane D.; Ponsardin, Patrick; Hueser, Alene W.

    1994-01-01

    An airborne differential absorption lidar (DIAL) system has been developed at the NASA Langley Research Center for remote measurements of atmospheric water vapor (H2O) and aerosols. A solid-state alexandrite laser with a 1-pm linewidth and greater than 99.85% spectral purity was used as the on-line transmitter. Solid-state avalanche photodiode detector technology has replaced photomultiplier tubes in the receiver system, providing an average increase by a factor of 1.5-2.5 in the signal-to-noise ratio of the H2O measurement. By incorporating advanced diagnostic and data-acquisition instrumentation into other subsystems, we achieved additional improvements in system operational reliability and measurement accuracy. Laboratory spectroscopic measurements of H2O absorption-line parameters were performed to reduce the uncertainties in our knowledge of the absorption cross sections. Line-center H2O absorption cross sections were determined, with errors of 3-6%, for more than 120 lines in the 720-nm region. Flight tests of the system were conducted during 1989-1991 on the NASA Wallops Flight Facility Electra aircraft, and extensive intercomparison measurements were performed with dew-point hygrometers and H2O radiosondes. The H2O distributions measured with the DIAL system differed by less than 10% from the profiles determined with the in situ probes in a variety of atmospheric conditions.

  8. Identification and Quantitative Measurements of Chemical Species by Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Zondlo, Mark A.; Bomse, David S.

    2005-01-01

    The development of a miniature gas chromatograph/mass spectrometer system for the measurement of chemical species of interest to combustion is described. The completed system is a fully-contained, automated instrument consisting of a sampling inlet, a small-scale gas chromatograph, a miniature, quadrupole mass spectrometer, vacuum pumps, and software. A pair of computer-driven valves controls the gas sampling and introduction to the chromatographic column. The column has a stainless steel exterior and a silica interior, and contains an adsorbent of that is used to separate organic species. The detection system is based on a quadrupole mass spectrometer consisting of a micropole array, electrometer, and a computer interface. The vacuum system has two miniature pumps to maintain the low pressure needed for the mass spectrometer. A laptop computer uses custom software to control the entire system and collect the data. In a laboratory demonstration, the system separated calibration mixtures containing 1000 ppm of alkanes and alkenes.

  9. A benchmarking method to measure dietary absorption efficiency of chemicals by fish.

    PubMed

    Xiao, Ruiyang; Adolfsson-Erici, Margaretha; Åkerman, Gun; McLachlan, Michael S; MacLeod, Matthew

    2013-12-01

    Understanding the dietary absorption efficiency of chemicals in the gastrointestinal tract of fish is important from both a scientific and a regulatory point of view. However, reported fish absorption efficiencies for well-studied chemicals are highly variable. In the present study, the authors developed and exploited an internal chemical benchmarking method that has the potential to reduce uncertainty and variability and, thus, to improve the precision of measurements of fish absorption efficiency. The authors applied the benchmarking method to measure the gross absorption efficiency for 15 chemicals with a wide range of physicochemical properties and structures. They selected 2,2',5,6'-tetrachlorobiphenyl (PCB53) and decabromodiphenyl ethane as absorbable and nonabsorbable benchmarks, respectively. Quantities of chemicals determined in fish were benchmarked to the fraction of PCB53 recovered in fish, and quantities of chemicals determined in feces were benchmarked to the fraction of decabromodiphenyl ethane recovered in feces. The performance of the benchmarking procedure was evaluated based on the recovery of the test chemicals and precision of absorption efficiency from repeated tests. Benchmarking did not improve the precision of the measurements; after benchmarking, however, the median recovery for 15 chemicals was 106%, and variability of recoveries was reduced compared with before benchmarking, suggesting that benchmarking could account for incomplete extraction of chemical in fish and incomplete collection of feces from different tests.

  10. Near-IR diode laser absorption for measurement of tropospheric HO2

    NASA Technical Reports Server (NTRS)

    Stanton, Alan C.

    1994-01-01

    The possibility of using tunable lead salt diode lasers in the infrared for measurement of tropospheric HO2 has been frequently considered. Although the sensitivity of diode laser absorption has been improved through the use of high frequency detection techniques, nature has been unkind in that the HO2 absorption cross sections are weak. Even using the most optimistic assumptions about attainable path length and detectable absorbance, measurement of tropospheric HO2 by diode laser absorption in the mid-IR appears marginal. A possible alternative method for measuring HO2 is by absorption at near-infrared wavelengths. Several absorption bands of HO2 occur in the wavelength region between 1.2 and 1.6 micron due to electronic transitions and overtones of the fundamental vibrational modes. InGaAsP diode lasers operate in this wavelength region and can be used for high resolution spectroscopy in a manner analogous to the lead salt lasers. A diode laser system in the near-IR offers some advantages.

  11. Measurement and feature analysis of absorption spectra of four algal species

    NASA Astrophysics Data System (ADS)

    Zhu, Jianhua; Zhou, Hongli; Han, Bing; Li, Tongji

    2016-04-01

    Two methods for particulate pigments (i.e., quantitative filter technique, QFT, and in vivo measurement, InVivo, respectively) and two methods for dissolved pigments (i.e., Acetone Extracts, AceEx, and high-performance liquid chromatography, HPLC, respectively) were used to obtain the optical absorption coefficient spectra for cultures of four typical algal species. Through normalization and analysis of the spectra, it is shown that (1) the four methods are able to measure optical absorption spectra of particulate and/or dissolved pigments; (2) that the optical absorption spectra of particulate and dissolved pigments were consistent in terms of the peak position in the blue wavelength, and the difference of the peak position in the near infrared wavelength was ~10 nm between each other; and (3) that the leveling effect of the absorption spectra of particulate pigments was significant. These four methods can all effectively measure the absorption coefficients of phytoplankton pigments, while each one has its unique advantages in different applications. Therefore, appropriate method should be carefully selected for various application due to their intrinsic difference.

  12. Measurement and feature analysis of absorption spectra of four algal species

    NASA Astrophysics Data System (ADS)

    Zhu, Jianhua; Zhou, Hongli; Han, Bing; Li, Tongji

    2017-03-01

    Two methods for particulate pigments (i.e., quantitative filter technique, QFT, and in vivo measurement, InVivo, respectively) and two methods for dissolved pigments (i.e., Acetone Extracts, AceEx, and high-performance liquid chromatography, HPLC, respectively) were used to obtain the optical absorption coefficient spectra for cultures of four typical algal species. Through normalization and analysis of the spectra, it is shown that (1) the four methods are able to measure optical absorption spectra of particulate and/or dissolved pigments; (2) that the optical absorption spectra of particulate and dissolved pigments were consistent in terms of the peak position in the blue wavelength, and the difference of the peak position in the near infrared wavelength was 10 nm between each other; and (3) that the leveling effect of the absorption spectra of particulate pigments was significant. These four methods can all effectively measure the absorption coefficients of phytoplankton pigments, while each one has its unique advantages in different applications. Therefore, appropriate method should be carefully selected for various application due to their intrinsic difference.

  13. Deriving brown carbon from multiwavelength absorption measurements: method and application to AERONET and Aethalometer observations

    NASA Astrophysics Data System (ADS)

    Wang, Xuan; Heald, Colette L.; Sedlacek, Arthur J.; de Sá, Suzane S.; Martin, Scot T.; Lizabeth Alexander, M.; Watson, Thomas B.; Aiken, Allison C.; Springston, Stephen R.; Artaxo, Paulo

    2016-10-01

    The radiative impact of organic aerosols (OA) is a large source of uncertainty in estimating the global direct radiative effect (DRE) of aerosols. This radiative impact includes not only light scattering but also light absorption from a subclass of OA referred to as brown carbon (BrC). However, the absorption properties of BrC are poorly understood, leading to large uncertainties in modeling studies. To obtain observational constraints from measurements, a simple absorption Ångström exponent (AAE) method is often used to separate the contribution of BrC absorption from that of black carbon (BC). However, this attribution method is based on assumptions regarding the spectral dependence of BC that are often violated in the ambient atmosphere. Here we develop a new AAE method which improves upon previous approaches by using the information from the wavelength-dependent measurements themselves and by allowing for an atmospherically relevant range of BC properties, rather than fixing these at a single assumed value. We note that constraints on BC optical properties and mixing state would help further improve this method. We apply this method to multiwavelength absorption aerosol optical depth (AAOD) measurements at AERONET sites worldwide and surface aerosol absorption measurements at multiple ambient sites. We estimate that BrC globally contributes up to 40 % of the seasonally averaged absorption at 440 nm. We find that the mass absorption coefficient of OA (OA-MAC) is positively correlated with the BC / OA mass ratio. Based on the variability in BC properties and BC / OA emission ratio, we estimate a range of 0.05-1.5 m2 g-1 for OA-MAC at 440 nm. Using the combination of AERONET and OMI UV absorption observations we estimate that the AAE388/440 nm for BrC is generally ˜ 4 worldwide, with a smaller value in Europe (< 2). Our analyses of observations at two surface sites (Cape Cod, to the southeast of Boston, and the GoAmazon2014/5 T3 site, to the west of

  14. Photon burst mass spectrometry for the measurement of {sup 85}Kr at ambient levels

    SciTech Connect

    Fairbank, W.M. Jr.; LaBelle, R.D.; Hansen, C.S.

    1998-12-01

    Photon Burst Mass Spectrometry has been used to measure {sup 85}Kr in a sample with an abundance of 6 x 10{sup {minus}9}. Improvements in detection efficiency by the use of avalanche photodiodes cooled to liquid nitrogen temperature are reported, which should make possible measurement of {sup 85}Kr at the ambient atmospheric abundance of 10{sup {minus}11}. Potential applications include nuclear monitoring, atmospheric transport, and dating young ground water up to 40 years.

  15. Attogram measurement of rare isotopes by CW resonance ionization mass spectrometry

    SciTech Connect

    Bushaw, B.A.

    1992-05-01

    Three-color double-resonance ionization mass spectrometry, using two single-frequency cw dye lasers and a cw carbon dioxide laser, has been applied to the detection of attogram quantities of rare radionuclides. {sup 210}Pb has been measured in human hair and brain tissue samples to assess indoor radon exposure. Measurements on {sup 90}Sr have shown overall isotopic selectivity of greater than 10{sup 9} despite unfavorable isotope shifts relative to the major stable isotope, {sup 88}Sr.

  16. Cavity ring-down spectroscopy (CRDS) system for measuring atmospheric mercury using differential absorption

    NASA Astrophysics Data System (ADS)

    Pierce, A.; Obrist, D.; Moosmuller, H.; Moore, C.

    2012-04-01

    Atmospheric elemental mercury (Hg0) is a globally pervasive element that can be transported and deposited to remote ecosystems where it poses — particularly in its methylated form — harm to many organisms including humans. Current techniques for measurement of atmospheric Hg0 require several liters of sample air and several minutes for each analysis. Fast-response (i.e., 1 second or faster) measurements would improve our ability to understand and track chemical cycling of mercury in the atmosphere, including high frequency Hg0 fluctuations, sources and sinks, and chemical transformation processes. We present theory, design, challenges, and current results of our new prototype sensor based on cavity ring-down spectroscopy (CRDS) for fast-response measurement of Hg0 mass concentrations. CRDS is a direct absorption technique that implements path-lengths of multiple kilometers in a compact absorption cell using high-reflectivity mirrors, thereby improving sensitivity and reducing sample volume compared to conventional absorption spectroscopy. Our sensor includes a frequency-doubled, dye-laser emitting laser pulses tunable from 215 to 280 nm, pumped by a Q-switched, frequency tripled Nd:YAG laser with a pulse repetition rate of 50 Hz. We present how we successfully perform automated wavelength locking and stabilization of the laser to the peak Hg0 absorption line at 253.65 nm using an external isotopically-enriched mercury (202Hg0) cell. An emphasis of this presentation will be on the implementation of differential absorption measurement whereby measurements are alternated between the peak Hg0 absorption wavelength and a nearby wavelength "off" the absorption line. This can be achieved using a piezo electric tuning element that allows for pulse-by-pulse tuning and detuning of the laser "online" and "offline" of the Hg absorption line, and thereby allows for continuous correction of baseline extinction losses. Unexpected challenges with this approach included

  17. Developments in Methods for Measuring the Intestinal Absorption of Nanoparticle-Bound Drugs

    PubMed Central

    Liu, Wei; Pan, Hao; Zhang, Caiyun; Zhao, Liling; Zhao, Ruixia; Zhu, Yongtao; Pan, Weisan

    2016-01-01

    With the rapid development of nanotechnology, novel drug delivery systems comprising orally administered nanoparticles (NPs) have been paid increasing attention in recent years. The bioavailability of orally administered drugs has significant influence on drug efficacy and therapeutic dosage, and it is therefore imperative that the intestinal absorption of oral NPs be investigated. This review examines the various literature on the oral absorption of polymeric NPs, and provides an overview of the intestinal absorption models that have been developed for the study of oral nanoparticles. Three major categories of models including a total of eight measurement methods are described in detail (in vitro: dialysis bag, rat gut sac, Ussing chamber, cell culture model; in situ: intestinal perfusion, intestinal loops, intestinal vascular cannulation; in vivo: the blood/urine drug concentration method), and the advantages and disadvantages of each method are contrasted and elucidated. In general, in vitro and in situ methods are relatively convenient but lack accuracy, while the in vivo method is troublesome but can provide a true reflection of drug absorption in vivo. This review summarizes the development of intestinal absorption experiments in recent years and provides a reference for the systematic study of the intestinal absorption of nanoparticle-bound drugs. PMID:27455239

  18. Developments in Methods for Measuring the Intestinal Absorption of Nanoparticle-Bound Drugs.

    PubMed

    Liu, Wei; Pan, Hao; Zhang, Caiyun; Zhao, Liling; Zhao, Ruixia; Zhu, Yongtao; Pan, Weisan

    2016-07-21

    With the rapid development of nanotechnology, novel drug delivery systems comprising orally administered nanoparticles (NPs) have been paid increasing attention in recent years. The bioavailability of orally administered drugs has significant influence on drug efficacy and therapeutic dosage, and it is therefore imperative that the intestinal absorption of oral NPs be investigated. This review examines the various literature on the oral absorption of polymeric NPs, and provides an overview of the intestinal absorption models that have been developed for the study of oral nanoparticles. Three major categories of models including a total of eight measurement methods are described in detail (in vitro: dialysis bag, rat gut sac, Ussing chamber, cell culture model; in situ: intestinal perfusion, intestinal loops, intestinal vascular cannulation; in vivo: the blood/urine drug concentration method), and the advantages and disadvantages of each method are contrasted and elucidated. In general, in vitro and in situ methods are relatively convenient but lack accuracy, while the in vivo method is troublesome but can provide a true reflection of drug absorption in vivo. This review summarizes the development of intestinal absorption experiments in recent years and provides a reference for the systematic study of the intestinal absorption of nanoparticle-bound drugs.

  19. Sandwich concept: enhancement for direct absorption measurements by laser-induced deflection (LID) technique

    NASA Astrophysics Data System (ADS)

    Mühlig, Ch.; Bublitz, S.; Paa, W.

    2012-11-01

    The new sandwich concept for absolute photo-thermal absorption measurements using the laser induced deflection (LID) technique is introduced and tested in comparison to the standard LID concept. The sandwich concept's idea is the decoupling of the optical materials for the pump and probe beams by placing a sample of investigation in between two optical (sandwich) plates. The pump beam is guided through the sample whereas the probe beams are deflected within the sandwich plates by the thermal lens that is generated by heat transfer from the irradiated sample. Electrical simulation and laser experiments reveal that using appropriate optical materials for the sandwich plates, the absorption detection limit for photo-thermally insensitive materials can be lowered by up to two orders of magnitude. Another advantage of the sandwich concept, the shrinking of the currently required minimum sample size, was used to investigate the laser induced absorption change in a Nd:YVO4 crystal at 1030nm. It was found that the absorption in Nd:YVO4 lowers due to the laser irradiation but partially recovers during irradiation breaks. Furthermore, absorption spectroscopy has been performed at two LBO crystals in the wavelength range 410...600nm to study the absorption structure around the SHG wavelengths of common high power lasers based on Neodymium doped laser crystals.

  20. Integrating ion mobility spectrometry into mass spectrometry-based exposome measurements: what can it add and how far can it go?

    SciTech Connect

    Metz, Thomas O.; Baker, Erin S.; Schymanski, Emma L.; Renslow, Ryan S.; Thomas, Dennis G.; Causon, Tim J.; Webb, Ian K.; Hann, Stephan; Smith, Richard D.; Teeguarden, Justin G.

    2017-01-01

    Measuring the exposome remains a challenge due to the range and number of anthropogenic molecules that are encountered in our daily lives, as well as the complex systemic responses to these exposures. One option for improving the coverage, dynamic range and throughput of measurements is to incorporate ion mobility spectrometry (IMS) into current mass spectrometry (MS)-based analytical methods. In this perspective, we briefly review the state-of-the-art in measuring the exposome, and discuss the potential use for IMS-MS and the physico-chemical property of collisional cross section in both exposure assessment and molecular identification.

  1. Measurement of the depolarization ratio of Rayleigh scattering at absorption bands

    NASA Astrophysics Data System (ADS)

    Anglister, J.; Steinberg, I. Z.

    1981-01-01

    Measurements of the depolarization ratio ρv of light scattered by the pigments lycopene and β-carotene at the red part of their absorption bands yielded values which are very close to the theoretical value 1/3 of a fully anisotropic molecular polarizability, i.e., that due to an electric dipole moment. Measurements of ρv at the blue edge of the visible absorption band of pinacyanol chloride yielded a value of 0.75 at 472.2 nm, which is the maximum value that a depolarization ratio can assume, and is attained if the average molecular polarizability is zero. This is possible only if the diagonalized polarizability tensor has at least one negative element to counterbalance the positive ones. A negative refractive index at the blue edge of the absorption band is thus experimentally demonstrated.

  2. Airborne Carbon Dioxide Laser Absorption Spectrometer for IPDA Measurements of Tropospheric CO2: Recent Results

    NASA Technical Reports Server (NTRS)

    Spiers, Gary D.; Menzies, Robert T.

    2008-01-01

    The National Research Council's decadal survey on Earth Science and Applications from Space[1] recommended the Active Sensing of CO2 Emissions over Nights, Days, and Seasons (ASCENDS) mission for launch in 2013-2016 as a logical follow-on to the Orbiting Carbon Observatory (OCO) which is scheduled for launch in late 2008 [2]. The use of a laser absorption measurement technique provides the required ability to make day and night measurements of CO2 over all latitudes and seasons. As a demonstrator for an approach to meeting the instrument needs for the ASCENDS mission we have developed the airborne Carbon Dioxide Laser Absorption Spectrometer (CO2LAS) which uses the Integrated Path Differential Absorption (IPDA) Spectrometer [3] technique operating in the 2 micron wavelength region.. During 2006 a short engineering checkout flight of the CO2LAS was conducted and the results presented previously [4]. Several short flight campaigns were conducted during 2007 and we report results from these campaigns.

  3. Differences in molar absorptivity of 4-NP with the reaction solution and apparatus affect ALP measurement.

    PubMed

    Huang, W F; Yang, M Q; Zeng, J; Li, L Z; Cheng, G R

    1997-11-01

    We examined the differences in molar absorptivity of 4-NP obtained using different kits for ALP measurement and different instruments. The apparent molar absorptivity of 4-NP in the same reaction solution determined by six different instruments was 15.98, 16.72, 16.06, 17.00, 16.27, 17.62 and that using four different reaction solution kits for ALP with the same instrument was 16.90, 17.38, 17.72, 16.11. We measured ALP in three serum samples with six instruments using the same kit and in twelve serum samples with the same instrument using four kits. ALP activities measured using the same molar absorptivity value differed with the instrument(p < 0.01). However, those measured using the apparent molar absorptivity value for each instrument revealed no significant differences(p > 0.05). In conclusion, we suggest that standard material should be contained in each kit for enzyme measurement and the apparent epsilon for each kit and instrument should be obtained to minimize the systematic error caused by using the same epsilon in different laboratories.

  4. Sensitivity analysis of differential absorption lidar measurements in the mid-infrared region.

    PubMed

    Ambrico, P F; Amodeo, A; Di Girolamo, P; Spinelli, N

    2000-12-20

    The availability of new laser sources that are tunable in the IR spectral region opens new perspectives for differential absorption lidar (DIAL) measurements. A region of particular interest is located in the near IR, where some of the atmospheric pollutants have absorption lines that permit monitoring of emissions from industrial plants and in urban areas. In DIAL measurements, the absorption lines for the species to be measured must be carefully chosen to prevent interference from other molecules, to minimize the dependence of the absorption cross section on temperature, and to optimize the measurements with respect to the optical depth. We analyze the influence of these factors and discuss a set of criteria for selecting the best pairs of wavelengths (lambda(on) and lambda(off)) to be used in DIAL measurements of several molecular species (HCl, CO, CO(2), NO(2), CH(4), H(2)O, and O(2)). Moreover, a sensitivity study has been carried out for selected lines in three different regimes: clean air, urban polluted air, and emission from an incinerator stack.

  5. Improved And Quality Assessed Emission And Absorption Line Measurements In Sloan Digital Sky Survey Galaxies

    NASA Astrophysics Data System (ADS)

    Oh, Kyuseok; Sarzi, M.; Schawinski, K.; Yi, S. K.

    2011-01-01

    We have established a new database of absorption and emission line measurements from the Sloan Digital Sky Survey 7th data release for the galaxies within a redshift of 0.2. This work used publicly available codes, pPXF(penalized pixel-fitting) and GANDALF(gas and absorption line fitting), to achieve robust spectral fits and reliable measurements. The absorption line strengths measured by SDSS pipeline are seriously contaminated by emission fill-in. We effectively separate emission lines from absorption lines. For instance, this work successfully extract [NI] doublet from Mgb and it leads to more realistic result of alpha enhancement on late-type galaxies compared to the previous database. Besides accurately measuring line strengths, the database will be provided with new parameters that are indicative of line strength measurement quality. Users can build a subset of database optimal for their studies using specific cuts in the fitting quality parameters as well as empirical signal-to-noise. Applying these parameters, we found galaxies with dramatically broad line regions among the galaxies with poor fitting quality parameters. We applied a new continuum finding prescriptions to newly identified BLRs and they turned out to be Seyfert I nuclei.

  6. On-line UV-photooxidation with peroxodisulfate for automated flow injection and for high-performance liquid chromatography coupled to hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Tsalev, Dimiter L.; Sperling, Michael; Welz, Bernhard

    2000-04-01

    An automated on-line UV photooxidation with peroxodisulfate of some environmentally relevant organoarsenic and organotin compounds in a system built from commercially available modules has been studied and optimised with a view to both species-independent quantification of the total arsenic or tin in samples containing different organic species by flow injection hydride generation atomic absorption spectrometry (FI-HGAAS) and speciation analysis by coupled high-performance liquid chromatography (HPLC) with HGAAS detection. For organoarsenicals, the reaction with alkaline peroxodisulfate in a 10-15-m knotted reactor for >1.5 min insures >90% transformation of inorganic As(III) and six organoarsenic species to arsenate: monomethylarsonate, dimethylarsinate, arsenobetaine, arsenocholine, trimethylarsine oxide and tetramethylarsonium. For organotins, the UV photooxidation with acidic peroxodisulfate at 95-100°C provides recoveries of >80% for the inorganic tin, dimethyltin, trimethyltin, triethyltin, tripropyltin, triphenyltin, monobutyltin, dibutyltin and tributyltin but only approximately 15% for tetrabutyltin. The best characteristic masses in integrated absorbance ( Aint) and peak-height ( Ap) measurements, respectively, are 30 pg and 480 pg for arsenic(V) and 22 pg and 410 pg for tin(IV), employing 100-μl injections. The RSDs are 5.5% and 8.5% at 5 ng As(V) levels and 4.3% and 6.4% at 10 ng Sn(IV) levels in Aint and Ap modes, respectively. The limits of detection (LOD, 3σ) for As are 7 μg l -1 and 4 μg l -1 in FI-UV-HGAAS and HPLC-UV-HGAAS, respectively. The LODs for i-Sn(IV) are 2 μg l -1 in FI-UV-HGAAS, with both Aint and Ap measurements. The sample throughput rates are 20 and 12 samples per hour with 10-m and 15-m knotted reactors (i.d. 0.5 mm), respectively. Urine certified reference materials containing 0.052-0.48 μg ml -1 As have been analysed for their total arsenic content.

  7. Water vapour foreign-continuum absorption in near-infrared windows from laboratory measurements.

    PubMed

    Ptashnik, Igor V; McPheat, Robert A; Shine, Keith P; Smith, Kevin M; Williams, R Gary

    2012-06-13

    For a long time, it has been believed that atmospheric absorption of radiation within wavelength regions of relatively high infrared transmittance (so-called 'windows') was dominated by the water vapour self-continuum, that is, spectrally smooth absorption caused by H(2)O--H(2)O pair interaction. Absorption due to the foreign continuum (i.e. caused mostly by H(2)O--N(2) bimolecular absorption in the Earth's atmosphere) was considered to be negligible in the windows. We report new retrievals of the water vapour foreign continuum from high-resolution laboratory measurements at temperatures between 350 and 430 K in four near-infrared windows between 1.1 and 5 μm (9000-2000 cm(-1)). Our results indicate that the foreign continuum in these windows has a very weak temperature dependence and is typically between one and two orders of magnitude stronger than that given in representations of the continuum currently used in many climate and weather prediction models. This indicates that absorption owing to the foreign continuum may be comparable to the self-continuum under atmospheric conditions in the investigated windows. The calculated global-average clear-sky atmospheric absorption of solar radiation is increased by approximately 0.46 W m(-2) (or 0.6% of the total clear-sky absorption) by using these new measurements when compared with calculations applying the widely used MTCKD (Mlawer-Tobin-Clough-Kneizys-Davies) foreign-continuum model.

  8. Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces--A review.

    PubMed

    Welz, Bernhard; Lepri, Fábio G; Araujo, Rennan G O; Ferreira, Sérgio L C; Huang, Mao-Dong; Okruss, Michael; Becker-Ross, Helmut

    2009-08-11

    The literature about the investigation of molecular spectra of phosphorus, sulfur and the halogens in flames and furnaces, and the use of these spectra for the determination of these non-metals has been reviewed. Most of the investigations were carried out using conventional atomic absorption spectrometers, and there were in essence two different approaches. In the first one, dual-channel spectrometers with a hydrogen or deuterium lamp were used, applying the two-line method for background correction; in the second one, a line source was used that emitted an atomic line, which overlapped with the molecular spectrum. The first approach had the advantage that any spectral interval could be accessed, but it was susceptible to spectral interference; the second one had the advantage that the conventional background correction systems could be used to minimize spectral interferences, but had the problem that an atomic line had to be found, which was overlapping sufficiently well with the maximum of the molecular absorption spectrum. More recently a variety of molecular absorption spectra were investigated using a low-resolution polychromator with a CCD array detector, but no attempt was made to use this approach for quantitative determination of non-metals. The recent introduction and commercial availability of high-resolution continuum source atomic absorption spectrometers is offering completely new possibilities for molecular absorption spectrometry and its use for the determination of non-metals. The use of a high-intensity continuum source together with a high-resolution spectrometer and a CCD array detector makes possible selecting the optimum wavelength for the determination and to exclude most spectral interferences.

  9. Measurement of 151Sm with the HI-13 accelerator mass spectrometry system

    NASA Astrophysics Data System (ADS)

    Yin, Xinyi; He, Ming; Dong, Kejun; Wu, Shaoyong; Zhang, Jinsong; Zhang, Jilong; Wang, Tongxin; Cui, Anzhi; Ouyang, Yinggen; Zhang, Zhiyong; Yuan, Jian; Jiang, Shan

    2010-05-01

    151Sm is an interesting nuclide in many research fields. Measurement methods of the long-lived 151Sm with accelerator mass spectrometry have been developed at China Institute of Atomic Energy. The chemical form of samples was Sm 2O 3 and the extracted ion was SmO -. To date, the sensitivity, that is, the isotopic ratio, of 151Sm measured using accelerator mass spectrometry is about 10 -8. This method was also used to measure the concentration of tracer 151Sm in biological samples for clarifying whether the rare earth elements can enter into the brain. It is not possible at present to determine whether the tracer has penetrated the blood-brain barrier into the brain.

  10. Laser ablation inductively coupled plasma mass spectrometry measurement of isotope ratios in depleted uranium contaminated soils.

    PubMed

    Seltzer, Michael D

    2003-09-01

    Laser ablation of pressed soil pellets was examined as a means of direct sample introduction to enable inductively coupled plasma mass spectrometry (ICP-MS) screening of soils for residual depleted uranium (DU) contamination. Differentiation between depleted uranium, an anthropogenic contaminant, and naturally occurring uranium was accomplished on the basis of measured 235U/238U isotope ratios. The amount of sample preparation required for laser ablation is considerably less than that typically required for aqueous sample introduction. The amount of hazardous laboratory waste generated is diminished accordingly. During the present investigation, 235U/238U isotope ratios measured for field samples were in good agreement with those derived from gamma spectrometry measurements. However, substantial compensation was required to mitigate the effects of impaired pulse counting attributed to sample inhomogeneity and sporadic introduction of uranium analyte into the plasma.

  11. Liquid chromatography-electrothermal atomic absorption spectrometry for the separation and preconcentration of molybdenum in milk and infant formulas.

    PubMed

    López-García, I; Viñas, P; Romero-Romero, R; Hernández-Córdoba, M

    2007-08-06

    Two procedures for the electrothermal atomic absorption spectrometric determination of molybdenum in milk and infant formulas using slurried samples are described. For powdered milk samples, 10% (m/v) slurries were prepared in a medium containing 25 and 75% (v/v) concentrated hydrogen peroxide and hydrofluoric acid, respectively, and introduced directly into the furnace. Palladium (200 microg mL(-1)) was used as the modifier and calibration was carried out using aqueous standards prepared in the same medium. The detection limit was 0.02 microg g(-1) for powdered milk samples suspended at 10% (m/v) (equivalent to 2 microg L(-1)). The relative standard deviation (R.S.D.) for five measurements was 1.9%, the characteristic mass being 25 pg. For liquid milk samples, a procedure was proposed based on preconcentration and removal of the matrix, using ionic exchange (Amberlite IRA 743) and elution of molybdenum with 5% (m/v) NaOH. In this case, a 30-fold improvement in the calibration slope was achieved, leading to a detection limit of 0.04 microg L(-1) for liquid samples diluted to 10%. The R.S.D. was 3.5%. Using a size-based separation procedure, it was found that molybdenum is present in its inorganic form or associated to low molecular weight substances in cow milk, while in breast milk it is associated to proteins. The reliability of the procedure was checked by comparing the results obtained with those found using a previous mineralization stage and by analyzing three certified reference materials, namely, BCR 063R (skim milk powder), NBS 1549 (non-fat milk powder) and NBS 8435 (whole milk powder).

  12. A medium-throughput functional assay of KCNQ2 potassium channels using rubidium efflux and atomic absorption spectrometry.

    PubMed

    Scott, Clay W; Wilkins, Deidre E; Trivedi, Shephali; Crankshaw, Denis J

    2003-08-15

    Heterologous expression of KCNQ2 (Kv7.2) results in the formation of a slowly activating, noninactivating, voltage-gated potassium channel. Using a cell line that stably expresses KCNQ2, we developed a rubidium flux assay to measure the functional activity and pharmacological modulation of this ion channel. Rubidium flux was performed in a 96-well microtiter plate format; rubidium was quantified using an automated atomic absorption spectrometer to enable screening of 1000 data points/day. Cells accumulated rubidium at 37 degrees C in a monoexponential manner with t(1/2)=40min. Treating cells with elevated extracellular potassium caused membrane depolarization and stimulation of rubidium efflux through KCNQ2. The rate of rubidium efflux increased with increasing extracellular potassium: the t(1/2) at 50mM potassium was 5.1 min. Potassium-stimulated efflux was potentiated by the anticonvulsant drug retigabine (EC(50)=0.5 microM). Both potassium-induced and retigabine-facilitated efflux were blocked by TEA (IC(50)s=0.4 and 0.3mM, respectively) and the neurotransmitter release enhancers and putative cognition enhancers linopirdine (IC(50)s=2.3 and 7.1 microM, respectively) and XE991 (IC(50)s=0.3 and 0.9 microM, respectively). Screening a collection of ion channel modulators revealed additional inhibitors including clofilium (IC(50) = 27 microM). These studies extend the pharmacological profile of KCNQ2 and demonstrate the feasibility of using this assay system to rapidly screen for compounds that modulate the function of KCNQ2.

  13. A flow-batch internal standard procedure for iron determination in hydrated ethanol fuel by flame atomic absorption spectrometry.

    PubMed

    da Silva, José Edson; da Silva, Fábio André; Pimentel, M Fernanda; Honorato, Ricardo Saldanha; da Silva, Valdinete Lins; Montenegro, Maria da Conceição B S M; Araújo, Alberto N

    2006-10-15

    A flow-batch manifold coupled to a flame atomic absorption spectrometer was evaluated to assess the iron content by the internal standard method in hydrated ethanol used as fuel in automotive industry. For this assessment official methods require calibration procedures with matrix matching, making it difficult to obtain accurate results for samples adulterated by the addition of water. Nickel was selected as the internal standard since it is usually absent in samples and because it requires similar conditions of atomization. After procedure optimization, which requires about 4.25mL of sample and standard per measurement, it was possible to get linear analytical response for iron concentrations between 0.12 and 1.40mgL(-1) and a detection limit of 0.04mgL(-1). Eighteen samples were collected randomly from fuel stations in Pernambuco (Brazil) and iron concentration was determined using the proposed procedure. Comparison of results obtained (0.20-1.50mgL(-1)) showed a mean standard error of 3.9%, with 3.8% and 2.3% calculated for the mean variation coefficients of the proposed method and the reference procedure, respectively. For adulterated samples (0.12-0.64mgL(-1)), the mean standard error was 4.8% when compared with the standard addition method. These results allowed concluding that the proposed procedure is adequate to accomplish the determination of iron in ethanol fuel in a large scale basis with a sampling rate of about 10h(-1).

  14. Aerosol absorption measurement with a sinusoidal phase modulating fiber optic photo thermal interferometer

    NASA Astrophysics Data System (ADS)

    Li, Shuwang; Shao, Shiyong; Mei, Haiping; Rao, Ruizhong

    2016-10-01

    Aerosol light absorption plays an important role in the earth's atmosphere direct and semi-direct radiate forcing, simultaneously, it also has a huge influence on the visibility impairment and laser engineering application. Although various methods have been developed for measuring aerosol light absorption, huge challenge still remains in precision, accuracy and temporal resolution. The main reason is that, as a part of aerosol light extinction, aerosol light absorption always generates synchronously with aerosol light scattering, and unfortunately aerosol light scattering is much stronger in most cases. Here, a novel photo-thermal interferometry is proposed only for aerosol absorption measurement without disturbance from aerosol scattering. The photo-thermal interferometry consists of a sinusoidal phase-modulating single mode fiber-optic interferometer. The thermal dissipation, caused by aerosol energy from photo-thermal conversion when irritated by pump laser through interferometer, is detected. This approach is completely insensitive to aerosol scattering, and the single mode fiber-optic interferometer is compact, low-cost and insensitive to the polarization shading. The theory of this technique is illustrated, followed by the basic structure of the sinusoidal phase-modulating fiber-optic interferometer and demodulation algorithms. Qualitative and quantitative analysis results show that the new photo-thermal interference is a potential approach for aerosol absorption detection and environmental pollution detection.

  15. O absorption measurements in an engineering-scale high-pressure coal gasifier

    NASA Astrophysics Data System (ADS)

    Sun, Kai; Sur, Ritobrata; Jeffries, Jay B.; Hanson, Ronald K.; Clark, Tommy; Anthony, Justin; Machovec, Scott; Northington, John

    2014-10-01

    A real-time, in situ water vapor (H2O) sensor using a tunable diode laser near 1,352 nm was developed to continuously monitor water vapor in the synthesis gas of an engineering-scale high-pressure coal gasifier. Wavelength-scanned wavelength-modulation spectroscopy with second harmonic detection (WMS-2 f) was used to determine the absorption magnitude. The 1 f-normalized, WMS-2 f signal (WMS-2 f/1 f) was insensitive to non-absorption transmission losses including beam steering and light scattering by the particulate in the synthesis gas. A fitting strategy was used to simultaneously determine the water vapor mole fraction and the collisional-broadening width of the transition from the scanned 1 f-normalized WMS-2 f waveform at pressures up to 15 atm, which can be used for large absorbance values. This strategy is analogous to the fitting strategy for wavelength-scanned direct absorption measurements. In a test campaign at the US National Carbon Capture Center, the sensor demonstrated a water vapor detection limit of ~800 ppm (25 Hz bandwidth) at conditions with more than 99.99 % non-absorption transmission losses. Successful unattended monitoring was demonstrated over a 435 h period. Strong correlations between the sensor measurements and transient gasifier operation conditions were observed, demonstrating the capability of laser absorption to monitor the gasification process.

  16. Measurements and Modeling of Aerosol Absorption and Single Scattering Albedo at Ambient Relative Hum

    NASA Technical Reports Server (NTRS)

    Redemann, J.; Russell, P. B.; Hamill, P.

    2000-01-01

    Uncertainties in the aerosol single scattering albedo have been identified to be an important source of errors in current large-scale model estimates of the direct aerosol radiative forcing of climate. A number of investigators have obtained estimates of the single scattering albedo from a variety of remote sensing and in situ measurements during aerosol field experiments. During the Tropospheric Aerosol Radiative Forcing Observational Experiment (TARFOX, 1996) for example, estimates of the aerosol single scattering albedo were obtained (1) as a best-fit parameter in comparing radiative flux changes measured by airborne pyranometer to those computed from independently measured aerosol properties; (2) from estimates of the aerosol complex index of refraction derived using a combination of airborne sunphotometer, lidar backscatter and in situ size distribution measurements; and (3) from airborne measurements of aerosol scattering and absorption using nephelometers and absorption photometers. In this paper, we briefly compare the results of the latter two methods for two TARFOX case studies, since those techniques provide height-resolved information about the aerosol single scattering albedo. Estimates of the aerosol single scattering albedo from nephelometer and absorption photometer measurements require knowledge of the scattering and absorption humidification (i.e., the increase in these properties in response to an increase in ambient relative humidity), since both measurements are usually carried out at a relative humidity different from the ambient atmosphere. In principle, the scattering humidification factor can be measured, but there is currently no technique widely available to measure the absorption of an aerosol sample as a function of relative humidity. Frequently, for lack of better knowledge, the absorption humidification is assumed to be unity (meaning that there is no change in aerosol absorption due to an increase in ambient relative humidity). This

  17. High sensitivity measurement of amino acid isotope enrichment using liquid chromatography-mass spectrometry.

    PubMed

    van Eijk, Hans M H; Wijnands, Karolina A P; Bessems, Babs A F M; Olde Damink, Steven W; Dejong, Cornelis H C; Poeze, Martijn

    2012-09-15

    Measurement of the incorporation or conversion of infused stable isotope enriched metabolites in vivo such as amino acids plays a key role in metabolic research. Specific routes are frequently probed in knockout mouse models limiting the available amount of sample. Although less precise as compared to combustion-isotope ratio mass spectrometry (C-IRMS), gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-mass spectrometry (LC-MS) techniques are therefore often the method of choice to measure isotopic enrichment of target metabolites. However, under conditions of metabolic depletion, the precision of these systems becomes limiting. In this paper, studies were performed to enhance the sensitivity and precision of isotope enrichment measurements using LC-MS. Ion-statistics and resolution were identified as critical factors for this application when using a linear trap mass spectrometer. The combination with an automated pre-column derivatization and a carefully selected solvent mix allowed us to measure isotopic enrichments down to 0.005% at plasma concentrations as low as 5 μmol/l, an improvement by a factor of 100 compared to alternative methods. The resulting method now allowed measurement of the in vivo conversion of the amino acid arginine into citrulline as a marker for the production of nitric oxide in an in vivo murine endotoxemia model with depleted plasma levels of arginine and citrulline.

  18. Atmospheric Solar Absorption measurements in the lowest 3-km of the atmosphere with small UAVs

    NASA Astrophysics Data System (ADS)

    Ramana, M. V.; Ramanathan, V.; Roberts, G.; Corrigan, C.; Nguyen, H. V.; McFarquhar, G.

    2007-12-01

    This paper reports unique measurements of atmospheric solar absorption and heating rates in the visible (0.4- 0.7 Ým) and broadband (0.3-2.8 Ým) spectral regions using vertically stacked multiple light weight autonomous unmanned aerial vehicles (UAVs) during the Maldives autonomous UAV campaign (MAC). The UAVs and ground based remote sensing instruments determined most of the parameters required for calculating the albedo and vertical distribution of solar fluxes. Measured fluxes have been compared with those derived from a Monte-Carlo radiative transfer algorithm which can incorporate both gaseous and aerosol components. The analysis focuses on a cloud-free day when the air was polluted due to long range transport from India, and the mean aerosol optical depth (AOD) was 0.31 and mean single scattering albedo was 0.92. The UAV measured absorption AOD was 0.019 which agreed within 20% of the value of 0.024 reported by a ground based instrument. The observed and simulated solar absorption agreed within 5% above 1.0 km and aerosol absorption accounted for 30% to 50% of the absorption depending upon the altitude and solar zenith angle. Thus there was no need to invoke anomalous or excess absorption or unknown physics in clear skies, provided we account for aerosol black carbon. The diurnal mean absorption values for altitudes between 0.5 and 3.0 km msl were observed to be 41¡Ó3 Wm-2 (1.5 K/day) in the broadband region and 8¡Ó2 Wm-2 (0.3 K/day) in the visible region. Future investigations into the atmospheric absorption in cloudy skies will characterize the spatial and temporal variation of the cloudy atmosphere in sufficient detail to simulate the vertical distribution of net solar fluxes to permit comparison with the collected radiative observations. This next phase will utilize 4 stacked UAVs to observe the extended cloud decks off the coast of California. A combination of observations and models will then be used to assess if the amount of solar absorption

  19. Supersonic Mass Flux Measurements via Tunable Diode Laser Absorption and Non-Uniform Flow Modeling

    NASA Technical Reports Server (NTRS)

    Chang, Leyen S.; Strand, Christopher L.; Jeffries, Jay B.; Hanson, Ronald K.; Diskin, Glenn S.; Gaffney, Richard L.; Capriotti, Diego P.

    2011-01-01

    Measurements of mass flux are obtained in a vitiated supersonic ground test facility using a sensor based on line-of-sight (LOS) diode laser absorption of water vapor. Mass flux is determined from the product of measured velocity and density. The relative Doppler shift of an absorption transition for beams directed upstream and downstream in the flow is used to measure velocity. Temperature is determined from the ratio of absorption signals of two transitions (lambda(sub 1)=1349 nm and lambda(sub 2)=1341.5 nm) and is coupled with a facility pressure measurement to obtain density. The sensor exploits wavelength-modulation spectroscopy with second-harmonic detection (WMS-2f) for large signal-to-noise ratios and normalization with the 1f signal for rejection of non-absorption related transmission fluctuations. The sensor line-of-sight is translated both vertically and horizontally across the test section for spatially-resolved measurements. Time-resolved measurements of mass flux are used to assess the stability of flow conditions produced by the facility. Measurements of mass flux are within 1.5% of the value obtained using a facility predictive code. The distortion of the WMS lineshape caused by boundary layers along the laser line-of-sight is examined and the subsequent effect on the measured velocity is discussed. A method for correcting measured velocities for flow non-uniformities is introduced and application of this correction brings measured velocities within 4 m/s of the predicted value in a 1630 m/s flow.

  20. Uranyl ion: A convenient standard for transient molar absorption coefficient measurements

    SciTech Connect

    Bakac, A.; Burrows, H.D.

    1997-12-01

    Transient absorption spectra of an aqueous solution of uranyl sulfate have been measured in the ultraviolet and visible spectra. The excited uranyl ion may be a convenient standard for actinometry and photoacoustic calorimetry. (AIP) {copyright} {ital 1997} {ital Society for Applied Spectroscopy}

  1. Developing and Validating Field Measurement Scales for Absorptive Capacity and Experienced Community of Practice

    ERIC Educational Resources Information Center

    Cadiz, David; Sawyer, John E.; Griffith, Terri L.

    2009-01-01

    Research on knowledge transfer in organizations has been hampered by the lack of tools yielding valid scores for studying critical constructs in concert. The authors developed survey measures of absorptive capacity (the ability to transform new knowledge into usable knowledge) and experienced community of practice (the extent to which a person is…

  2. A balloon ozone measurement utilizing an optical absorption cell and an ejector air sampler

    NASA Technical Reports Server (NTRS)

    Hilsenrath, E.; Ashenfelter, T. E.

    1976-01-01

    Stratospheric ozone was measured from a balloon utilizing an ultraviolet absorption cell. The ambient air was sampled by means of an aspirator attached to the output end of the optical cell. A nominal ozone distribution was obtained from 16 km to the float altitude of 38 km.

  3. Optimal frequency selection of multi-channel O2-band different absorption barometric radar for air pressure measurements

    NASA Astrophysics Data System (ADS)

    Lin, Bing; Min, Qilong

    2017-02-01

    Through theoretical analysis, optimal selection of frequencies for O2 differential absorption radar systems on air pressure field measurements is achieved. The required differential absorption optical depth between a radar frequency pair is 0.5. With this required value and other considerations on water vapor absorption and the contamination of radio wave transmission, frequency pairs of present considered radar system are obtained. Significant impacts on general design of differential absorption remote sensing systems are expected from current results.

  4. Cesium oscillator strengths measured with a multiple-path-length absorption cell

    NASA Technical Reports Server (NTRS)

    Exton, R. J.

    1976-01-01

    Absorption-oscillator-strength measurements for the principal series in cesium were measured using a multiple-path-length cell. The optical arrangement included a movable transverse path for checking the uniformity of the alkali density along the length of the cell and which also allowed strength measurements to be made simultaneously on both strong and weak lines. The strengths measured on the first 10 doublets indicate an increasing trend in the doublet ratio. The individual line strengths are in close agreement with the high resolution measurements of Pichler (1974) and with the calculations of Norcross (1973).

  5. Calculation spreadsheet for uncertainty estimation of measurement results in gamma-ray spectrometry and its validation for quality assurance purpose.

    PubMed

    Ceccatelli, Alessia; Dybdal, Ashild; Fajgelj, Ales; Pitois, Aurelien

    2017-03-03

    An Excel calculation spreadsheet has been developed to estimate the uncertainty of measurement results in γ-ray spectrometry. It considers all relevant uncertainty components and calculates the combined standard uncertainty of the measurement result. The calculation spreadsheet has been validated using two independent open access software and is available for download free of charge at: https://nucleus.iaea.org/rpst/ReferenceProducts/Analytical_Methods/index.htm. It provides a simple and easy-to-use template for estimating the uncertainty of γ-ray spectrometry measurement results and supports the radioanalytical laboratories seeking accreditation for their measurements using γ-ray spectrometry.

  6. Apparatus and method for measurement of weak optical absorptions by thermally induced laser pulsing

    DOEpatents

    Cremers, D.A.; Keller, R.A.

    1982-06-08

    The thermal lensing phenomenon is used as the basis for measurement of weak optical absorptions when a cell containing the sample to be investigated is inserted into a normally continuous-wave operation laser-pumped dye laser cavity for which the output coupler is deliberately tilted relative to intracavity circulating laser light, and pulsed laser output ensues, the pulsewidth of which can be rlated to the sample absorptivity by a simple algorithm or calibration curve. A minimum detection limit of less than 10/sup -5/ cm/sup -1/ has been demonstrated using this technique.

  7. Apparatus and method for measurement of weak optical absorptions by thermally induced laser pulsing

    DOEpatents

    Cremers, David A.; Keller, Richard A.

    1985-01-01

    The thermal lensing phenomenon is used as the basis for measurement of weak optical absorptions when a cell containing the sample to be investigated is inserted into a normally continuous-wave operation laser-pumped dye laser cavity for which the output coupler is deliberately tilted relative to intracavity circulating laser light, and pulsed laser output ensues, the pulsewidth of which can be related to the sample absorptivity by a simple algorithm or calibration curve. A minimum detection limit of less than 10.sup.-5 cm.sup.-1 has been demonstrated using this technique.

  8. A numerical study of a method for measuring the effective in situ sound absorption coefficient.

    PubMed

    Kuipers, Erwin R; Wijnant, Ysbrand H; de Boer, André

    2012-09-01

    The accuracy of a method [Wijnant et al., Proc. of ISMA 31, Leuven, Belgium (2010), Vol. 31] for measurement of the effective area-averaged in situ sound absorption coefficient is investigated. Based on a local plane wave assumption, this method can be applied to sound fields for which a model is not available. Investigations were carried out by means of finite element simulations for a typical case. The results show that the method is a promising method for determining the effective area-averaged in situ sound absorption coefficient in complex sound fields.

  9. Error Reduction Methods for Integrated-path Differential-absorption Lidar Measurements

    NASA Technical Reports Server (NTRS)

    Chen, Jeffrey R.; Numata, Kenji; Wu, Stewart T.

    2012-01-01

    We report new modeling and error reduction methods for differential-absorption optical-depth (DAOD) measurements of atmospheric constituents using direct-detection integrated-path differential-absorption lidars. Errors from laser frequency noise are quantified in terms of the line center fluctuation and spectral line shape of the laser pulses, revealing relationships verified experimentally. A significant DAOD bias is removed by introducing a correction factor. Errors from surface height and reflectance variations can be reduced to tolerable levels by incorporating altimetry knowledge and "log after averaging", or by pointing the laser and receiver to a fixed surface spot during each wavelength cycle to shorten the time of "averaging before log".

  10. Photothermal measurement of absorption and scattering losses in thin films excited by surface plasmons.

    PubMed

    Domené, Esteban A; Balzarotti, Francisco; Bragas, Andrea V; Martínez, Oscar E

    2009-12-15

    We present a novel noncontact, photothermal technique, based on the focus error signal of a commercial CD pickup head that allows direct determination of absorption in thin films. Combined with extinction methods, this technique yields the scattering contribution to the losses. Surface plasmon polaritons are excited using the Kretschmann configuration in thin Au films of varying thickness. By measuring the extinction and absorption simultaneously, it is shown that dielectric constants and thickness retrieval leads to inconsistencies if the model does not account for scattering.

  11. Measurement of optical absorption coefficient of bio-tissue at 532nm wavelength

    NASA Astrophysics Data System (ADS)

    Huang, Chuyun; Li, Zhengjia; Yao, Yucheng; He, Yanyan

    2007-05-01

    Laser technology has succeeded in medical application. High power 532nm laser has applied in prostate ablation and other clinic application. To understand optical property of bio-tissue at 532nm wavelength, a method of monitoring surface temperature was used to measure absorption coefficient of gall-stone, porcine liver and canine prostate. The absorption coefficient of gall-stone is about 62cm -1 at 532nm wavelength, and those of porcine liver and canine prostate are about 13cm -1 and 5.4cm -1, respectively. These results help to understand the optical property of bio-tissue and offer theoretic reference for optical dosimetry in clinic application.

  12. Improved measurement of the neutron absorption cross section for very low velocities

    NASA Astrophysics Data System (ADS)

    Schroffenegger, J.; Fierlinger, P.; Hollering, A.; Geltenbort, P.; Lauer, T.; Rauch, H.; Zechlau, T.

    2016-01-01

    The absorption cross section of natural Gd and isotopic enriched 157Gd for ultra-cold neutrons (UCN) as a function of the velocity has been measured within a time-of-flight-experiment. Particular attention is paid to small velocities in the region of a few m/s. This is intended to determine the validity of the 1 / v-law governing absorption cross sections in this region and the resulting divergence at v = 0. The experiment does not show any significant violation of 1 / v for v > 3 m /s.

  13. Apparatus and method for measurement of weak optical absorptions by thermally induced laser pulsing

    DOEpatents

    Cremers, D.A.; Keller, R.A.

    1985-10-01

    The thermal lensing phenomenon is used as the basis for measurement of weak optical absorptions when a cell containing the sample to be investigated is inserted into a normally continuous-wave operation laser-pumped dye laser cavity for which the output coupler is deliberately tilted relative to intracavity circulating laser light, and pulsed laser output ensues, the pulsewidth of which can be related to the sample absorptivity by a simple algorithm or calibration curve. A minimum detection limit of less than 10[sup [minus]5] cm[sup [minus]1] has been demonstrated using this technique. 6 figs.

  14. Absorption-mode Fourier transform mass spectrometry: the effects of apodization and phasing on modified protein spectra.

    PubMed

    Qi, Yulin; Li, Huilin; Wills, Rebecca H; Perez-Hurtado, Pilar; Yu, Xiang; Kilgour, David P A; Barrow, Mark P; Lin, Cheng; O'Connor, Peter B

    2013-06-01

    The method of phasing broadband Fourier transform ion cyclotron resonance (FT-ICR) spectra allows plotting the spectra in the absorption-mode; this new approach significantly improves the quality of the data at no extra cost. Herein, an internal calibration method for calculating the phase function has been developed and successfully applied to the top-down spectra of modified proteins, where the peak intensities vary by 100×. The result shows that the use of absorption-mode spectra allows more peaks to be discerned within the recorded data, and this can reveal much greater information about the protein and modifications under investigation. In addition, noise and harmonic peaks can be assigned immediately in the absorption-mode.

  15. Assimilation of real-time riometer measurements into models of 30 MHz polar cap absorption

    NASA Astrophysics Data System (ADS)

    Rogers, Neil Christopher; Honary, Farideh

    2015-04-01

    Space weather events may adversely affect high frequency (HF) radio propagation, hence the ability to provide nowcasting and forecasting of HF radio absorption is key for industries that rely on HF communications. This paper presents methods of assimilating 30 MHz radio absorption measurements into two types of ionospheric polar cap absorption (PCA) model to improve their performance as nowcasting tools. Type 1 models calculate absorption as m times the square root of the flux of solar protons above an energy threshold, Et. Measurements from 14 riometers during 94 solar proton events (1995-2010) are assimilated by optimising the day and night values of m by linear regression. Further non-linear optimisations are demonstrated in which parameters such as Et are also optimised and additional terms characterise local time and seasonal variations. These optimisations reduce RMS errors by up to 36%. Type 2 models incorporate altitude profiles of electron and neutral densities and electron temperatures. Here the scale height of the effective recombination coefficient profile in the D-region is optimised by regression. Furthermore, two published models of the rigidity cut-off latitude (CL) are assessed by comparison with riometer measurements. A small improvement in performance is observed by introducing a 3-h lag in the geomagnetic index Kp in the CL models. Assimilating data from a single riometer in the polar cap reduces RMS errors below 1 dB with less than 0.2 dB bias. However, many high-latitude riometers now provide absorption measurements in near-real time and we demonstrate how these data may be assimilated by fitting a low-order spherical harmonic function to both the measurements and a PCA model with optimised parameters.

  16. Differential Optical Absorption Spectroscopy (DOAS) using Targets: SO2 and NO2 Measurements in Montevideo City

    NASA Astrophysics Data System (ADS)

    Louban, Ilia; Píriz, Gustavo; Platt, Ulrich; Frins, Erna

    2008-04-01

    SO2 and NO2 were remotely measured in a main street of Montevideo city using Multiaxis-Differential Optical Absorption Spectroscopy (MAX-DOAS) combined with on-field selected targets. Target-based measurements are the basis of a new experimental procedure called Topographic Target Light scattering-DOAS (TOTAL-DOAS) that provides a well define absorption path to measure the near surface distribution of trace gases in the boundary layer. It combines the measurement principles of the long-path DOAS and zenith-scattered sunlight DOAS, within the near UV and VIS spectral range. We give a general description of the procedure and present first results of the 2006 campaign at Montevideo.

  17. Staying Alive: Measuring Intact Viable Microbes with Electrospray Ionization Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Forsberg, Erica; Fang, Mingliang; Siuzdak, Gary

    2017-01-01

    Mass spectrometry has traditionally been the technology of choice for small molecule analysis, making significant inroads into metabolism, clinical diagnostics, and pharmacodynamics since the 1960s. In the mid-1980s, with the discovery of electrospray ionization (ESI) for biomolecule analysis, a new door opened for applications beyond small molecules. Initially, proteins were widely examined, followed by oligonucleotides and other nonvolatile molecules. Then in 1991, three intriguing studies reported using mass spectrometry to examine noncovalent protein complexes, results that have been expanded on for the last 25 years. Those experiments also raised the questions: How soft is ESI, and can it be used to examine even more complex interactions? Our lab addressed these questions with the analyses of viruses, which were initially tested for viability following electrospray ionization and their passage through a quadrupole mass analyzer by placing them on an active medium that would allow them to propagate. This observation has been replicated on multiple different systems, including experiments on an even bigger microbe, a spore. The question of analysis was also addressed in the early 2000s with charge detection mass spectrometry. This unique technology could simultaneously measure mass-to-charge and charge, allowing for the direct determination of the mass of a virus. More recent experiments on spores and enveloped viruses have given us insight into the range of mass spectrometry's capabilities (reaching 100 trillion Da), beginning to answer fundamental questions regarding the complexity of these organisms beyond proteins and genes, and how small molecules are integral to these supramolecular living structures.

  18. Calculation of UV attenuation and colored dissolved organic matter absorption spectra from measurements of ocean color

    NASA Astrophysics Data System (ADS)

    Johannessen, S. C.; Miller, W. L.; Cullen, J. J.

    2003-09-01

    The absorption of ultraviolet and visible radiation by colored or chromophoric dissolved organic matter (CDOM) drives much of marine photochemistry. It also affects the penetration of ultraviolet radiation (UV) into the water column and can confound remote estimates of chlorophyll concentration. Measurements of ocean color from satellites can be used to predict UV attenuation and CDOM absorption spectra from relationships between visible reflectance, UV attenuation, and absorption by CDOM. Samples were taken from the Bering Sea and from the Mid-Atlantic Bight, and water types ranged from turbid, inshore waters to the Gulf Stream. We determined the following relationships between in situ visible radiance reflectance, Lu/Ed (λ) (sr-1), and diffuse attenuation of UV, Kd(λ) (m-1): Kd(323nm) = 0.781[Lu/Ed(412)/Lu/Ed(555)]-1.07; Kd(338nm) = 0.604[Lu/Ed(412)/Lu/Ed(555)]-1.12; Kd(380 nm) = 0.302[Lu/Ed(412)/Lu/Ed(555)]-1.24. Consistent with published observations, these empirical relationships predict that the spectral slope coefficient of CDOM absorption increases as diffuse attenuation of UV decreases. Excluding samples from turbid bays, the ratio of the CDOM absorption coefficient to Kd is 0.90 at 323 nm, 0.86 at 338 nm, and 0.97 at 380 nm. We applied these relationships to SeaWiFS images of normalized water-leaving radiance to calculate the CDOM absorption and UV attenuation in the Mid-Atlantic Bight in May, July, and August 1998. The images showed a decrease in UV attenuation from May to August of approximately 50%. We also produced images of the areal distribution of the spectral slope coefficient of CDOM absorption in the Georgia Bight. The spectral slope coefficient increased offshore and changed with season.

  19. A method for measuring magnetic fields in sunspots using Zeeman-broadened absorption lines

    NASA Astrophysics Data System (ADS)

    Oostra, Benjamin

    2017-04-01

    We present measurements of magnetic fields in several sunspots using high-resolution spectra obtained with the ESPARTACO spectrograph at the Universidad de los Andes, with the aim to explore experimental possibilities for students. Because the Zeeman line splitting is smaller than the line width, our work only observes broadened absorption lines. This broadening, however, can be measured and suitably modeled, giving realistic quantitative results.

  20. Combined laser calorimetry and photothermal technique for absorption measurement of optical coatings

    SciTech Connect

    Li Bincheng; Blaschke, Holger; Ristau, Detlev

    2006-08-10

    To the best of our knowledge, a combined sensitive technique employing both laser calorimetry and a surface thermal lens scheme for measuring absorption values of optical coatings is presented for the first time. Laser calorimetric and pulsed surface thermal lens signals are simultaneously obtained with a highly reflecting UV coating sample irradiated at 193 nm. The advantages and potential applications of the combined technique and the experimental factors limiting the measurement sensitivity are discussed.

  1. Combined laser calorimetry and photothermal technique for absorption measurement of optical coatings.

    PubMed

    Li, Bincheng; Blaschke, Holger; Ristau, Detlev

    2006-08-10

    To the best of our knowledge, a combined sensitive technique employing both laser calorimetry and a surface thermal lens scheme for measuring absorption values of optical coatings is presented for the first time. Laser calorimetric and pulsed surface thermal lens signals are simultaneously obtained with a highly reflecting UV coating sample irradiated at 193 nm. The advantages and potential applications of the combined technique and the experimental factors limiting the measurement sensitivity are discussed.

  2. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Orani, Anna Maria; Han, Eunmi; Mandjukov, Petko; Vassileva, Emilia

    2015-01-01

    Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

  3. Method development for the determination of cadmium in fertilizer samples using high-resolution continuum source graphite furnace atomic absorption spectrometry and slurry sampling

    NASA Astrophysics Data System (ADS)

    Borges, Aline R.; Becker, Emilene M.; Lequeux, Céline; Vale, Maria Goreti R.; Ferreira, Sergio L. C.; Welz, Bernhard

    2011-07-01

    The determination of cadmium (Cd) in fertilizers is of major interest, as this element can cause growth problems in plants, and also affect animals and humans. High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with charge-coupled device (CCD) array detection overcomes several of the limitations encountered with conventional line source AAS, especially the problem of accurate background measurement and correction. In this work an analytical method has been developed to determine Cd in fertilizer samples by HR-CS GF AAS using slurry sampling. Both a mixture of 10 μg Pd + 6 μg Mg in solution and 400 μg of iridium as permanent modifier have been investigated and aqueous standards were used for calibration. Pyrolysis and atomization temperatures were 600 °C and 1600 °C for the Pd-Mg modifier, and 500 °C and 1600 °C for Ir, respectively. The results obtained for Cd in the certified reference material NIST SRM 695 (Trace Elements in Multi-Nutrient Fertilizer) of 16.7 ± 1.3 μg g -1 and 16.4 ± 0.75 μg g -1 for the Pd-Mg and Ir modifier, respectively, were statistically not different from the certified value of 16.9 ± 0.2 μg g -1 on a 95% confidence level; however, the results obtained with the Ir modifier were significantly lower than those for the Pd-Mg modifier for most of the samples. The characteristic mass was 1.0 pg for the Pd-Mg modifier and 1.1 pg Cd for the Ir modifier, and the correlation coefficients (R 2) of the calibration were > 0.99. The instrumental limits of detection were 7.5 and 7.9 ng g -1, and the limits of quantification were 25 and 27 ng g -1 for Pd-Mg and Ir, respectively, based on a sample mass of 5 mg. The cadmium concentration in the investigated samples was between 0.07 and 5.5 μg g -1 Cd, and hence below the maximum value of 20 μg g -1 Cd permitted by Brazilian legislation.

  4. Metallomics approach to trace element analysis in ustilago maydis using cellular fractionation, atomic absorption spectrometry, and size exclusion chromatography with ICP-MS detection.

    PubMed

    Muñoz, Alma Hortensia Serafin; Kubachka, Kevin; Wrobel, Kazimierz; Corona, Felix Gutierrez; Yathavakilla, Santha K V; Caruso, Joseph A; Wrobel, Katarzyna

    2005-06-29

    Huitlacoche is the ethnic name of the young fruiting bodies of Ustilago maydis, a common parasite of maize. In Mexico and other Latin American countries, this fungus has been traditionally appreciated as a local delicacy. In this work a metallomics approach was used with the determination of eight elements in huitlacoche by electrothermal atomic absorption spectrometry as one facet of this approach. The results obtained indicated relatively lower concentrations of commonly analyzed metals, as referred to the data reported for other mushroom types. This effect was ascribed to different accessibilities of elements, depending on fungus substrate (lower from plant than from soil). Subcellular fractionation was accomplished by centrifugation of cell homogenates suspended in Tris-HCl buffer. Recoveries of the fractionation procedure were in the range of 71-103%. For six elements (Cr, Cu, Fe, Mn, Ni, and Pb), the mean relative contributions in cytosol, cell walls, and mixed membrane fraction were 50.7, 48.2, and 1.1% respectively. To attain the molecular weight distribution of compounds containing target elements as an additional aspect of the metallomics approach, the fungus extract (1% sodium dodecyl sulfate in Tris-HCl, 30 mmol L(-)(1), pH 7.0) was analyzed by size exclusion chromatography with UV and ICP-MS detection. With spectrophotometric detection (280 nm), the elution of high molecular weight compounds was observed in the form of one peak (MW > 10 kDa), and several lower peaks appeared at higher retention times (MW < 10 kDa). On ICP-MS chromatograms, a coelution of (59)Co, (63)Cu, (57)Fe, (202)Hg, (60)Ni, and (80)Se with the first peak on the UV chromatogram was clearly observed, indicating that a fraction of each element incorporated with high molecular weight compounds (12.7, 19.8, 33.7, 100, 19.4, and 45.8%, respectively, based on the peak area measurements). From a comparison of (80)Se and (33)S chromatograms (for sulfur analysis, the extract was obtained in

  5. [Study on Content Determination of Lead and Arsenic in Four Traditional Tibetan Medicine Prescription Preparations by Wet Digestion Flow Injection-Hydride Generation-Atomic Absorption Spectrometry].

    PubMed

    Zheng, Zhi-yuan; Du, Yu-zhi; Zhang, Ming; Yu, Ming-jie; Li, Cen; Yang, Hong-xia; Zhao, Jing; Xia, Zheng-hua; Wei, Li-xin

    2015-04-01

    Four common traditional tibetan medicine prescription preparations "Anzhijinghuasan, Dangzuo, Renqingchangjue and Rannasangpei" in tibetan areas were selected as study objects in the present study. The purpose was to try to establish a kind of wet digestion and flow injection-hydride generation-atomic absorption spectrometry (FI-HAAS) associated analysis method for the content determinations of lead and arsenic in traditional tibetan medicine under optimized digestion and measurement conditions and determine their contents accurately. Under these optimum operating conditions, experimental results were as follows. The detection limits for lead and arsenic were 0.067 and 0.012 µg · mL(-1) respectively. The quantification limits for lead and arsenic were 0.22 and 0.041 µg · mL(-1) respectively. The linear ranges for lead and arsenic were 25-1,600 ng · mL(-1) (r = 0.9995) and 12.5-800 ng · mL(-1) (r = 0.9994) respectively. The degrees of precision(RSD) for lead and arsenic were 2.0% and 3.2% respectively. The recovery rates for lead and arsenic were 98.00%-99.98% and 96.67%-99.87% respectively. The content determination results of lead and arsenic in four traditional tibetan medicine prescription preparations were as fol- lows. The contents of lead and arsenic in Anzhijinghuasan are 0.63-0.67 µg · g(-1) and 0.32-0.33 µg · g(-1) in Anzhijinghua- san, 42.92-43.36 µg · g(-1) and 24.67-25.87 µg · g(-1) in Dangzuo, 1,611. 39-1,631.36 µg · g(-1) and 926.76-956.52 µg- g(-1) in Renqing Changjue, and 1,102.28-1,119.127 µg-g(-1) and 509.96-516.87 µg · g(-1) in Rannasangpei, respectively. This study established a method for content determination of lead and arsenic in traditional tibetan medicine, and determined the content levels of lead and arsenic in four tibetan medicine-prescription preparations accurately. In addition, these results also provide the basis for the safe and effective use of those medicines in clinic.

  6. Retrieval of Black Carbon Absorption from Proposed Satellite Measurements Over the Ocean Glint

    NASA Technical Reports Server (NTRS)

    Kaufman, Y. J.; Matins, J. V.; Remer, L. A.; Schoeberl, M. R.; Yamasoe, M. A.; Lau, William K. M. (Technical Monitor)

    2001-01-01

    Haze and air pollution includes many chemicals that together form small particles suspended in the air called aerosols. One of the main ingredients found to affect climate and human health is Black Carbon. Black particles emitted from engines that do not burn the fuel completely, e.g. old trucks. Black carbon absorption of sunlight emerges as one of the key components of man-made forcing of climate. However, global characterization of black carbon emissions, distribution and pathways in which it can affect the amount of solar radiation absorbed by the atmosphere is very uncertain. A new method is proposed to measure sunlight absorption by fine aerosol particles containing black carbon over the ocean glint from a satellite mission designed for this purpose. The satellite will scan the same spot over the ocean in the glint plane and a plane 40 degrees off-glint a minute apart, collecting measurements of the reflected light across the solar spectrum. First the dark ocean off the glint is used to derive aerosol properties. Then the black carbon absorption is derived prop the attenuation of the bright glint by the aerosol layer. Such measurements if realized in a proposed future mission - COBRA are expected to produce global monthly climatology of black carbon absorption with high accuracy (110 to 15%) that can show their effect on climate.

  7. Measurement of the absorption rate of carbon dioxide into aqueous diethanolamine

    SciTech Connect

    Rowley, R.L.; Adams, M.E.; Marshall, T.L.; Oscarson, J.L.; Wilding, W.V.; Anderson, D.J.

    1998-05-01

    Aqueous alkanolamine solutions are commonly used in natural gas sweetening processes to remove the acid gases CO{sub 2} and H{sub 2}S. Absorption rates of gaseous CO{sub 2} into aqueous diethanolamine (DEA) solutions were measured in a quiescent, inverted-tube diffusiometer by monitoring the rate of pressure drop. The absorption rate was found to be insensitive to the diffusion coefficient of CO{sub 2} in solution but very sensitive to the diffusion rate of bicarbonate, protonated DEA, and carbamate ions. Evidence also suggested that chemical reaction equilibrium is rapid relative to diffusion. The diffusion coefficient of DEA in water was also measured using a Taylor dispersion apparatus. A numerical model was developed and used to regress diffusion coefficients of bicarbonate, carbamate, and protonated amine from measured absorption rates. CO{sub 2} absorption rates and diffusion coefficients of bicarbonate, carbamate, and protonated DEA were obtained at 298.2 K and 318.2 K in solutions containing 20, 35, and 50 mass % DEA in water.

  8. Inferring brown carbon content from UV aerosol absorption measurements during biomass burning season

    NASA Astrophysics Data System (ADS)

    Mok, J.; Krotkov, N. A.; Arola, A. T.; Torres, O.; Jethva, H. T.; Andrade, M.; Labow, G. J.; Eck, T. F.; Li, Z.; Dickerson, R. R.; Stenchikov, G. L.; Osipov, S.

    2015-12-01

    Measuring spectral dependence of light absorption by colored organic or "brown" carbon (BrC) is important, because of its effects on photolysis rates of ozone and surface ultraviolet (UV) radiation. Enhanced UV spectral absorption by BrC can in turn be exploited for simultaneous retrievals of BrC and black carbon (BC) column amounts in field campaigns. We present an innovative ground-based retrieval of BC and BrC volume fractions and their mass absorption efficiencies during the biomass burning season in Santa Cruz, Bolivia in September-October 2007. Our method combines retrieval of BC volume fraction using AERONET inversion in visible wavelengths with the inversion of total BC+BrC absorption (i.e., column effective imaginary refractive index, kmeas) using Diffuse/Direct irradiance measurements in UV wavelengths. First, we retrieve BrC volume fraction by fitting kmeas at 368nm using Maxwell-Garnett (MG) mixing rules assuming: (1) flat spectral dependence of kBC, (2) known value of kBrC at 368nm from laboratory absorption measurements or smoke chamber experiments, and (3) known BC volume fraction from AERONET inversion. Next, we derive kBrC in short UVB wavelengths by fitting kmeas at 305nm, 311nm, 317nm, 325nm, and 332nm using MG mixing rules and fixed volume fractions of BC and BrC. Our retrievals show larger than expected spectral dependence of kBrC in UVB wavelengths, implying reduced surface UVB irradiance and inhibited photolysis rates of surface ozone destruction. We use a one-dimensional chemical box model to show that the observed strong wavelength dependence of BrC absorption leads to inhibited photolysis of ozone to O(1D), a loss mechanism, while having little impact or even accelerating photolysis of NO2, an ozone production mechanism. Although BC only absorption in biomass burning aerosols is important for climate radiative forcing in the visible wavelengths, additional absorption by BrC is important because of its impact on surface UVB radiation

  9. Development of an alkali chloride vapour-generating apparatus for calibration of ultraviolet absorption measurements

    NASA Astrophysics Data System (ADS)

    Leffler, T.; Brackmann, C.; Berg, M.; Aldén, M.; Li, Z. S.

    2017-02-01

    A novel design of alkali chloride vapour-generating cell has been developed, which can serve as a calibration cell for quantitative ultraviolet absorption concentration measurements and meticulous spectral investigations of alkali compounds. The calibration cell was designed to provide alkali vapour of well-controlled concentrations and temperatures, and consisted of a sealed quartz cell measuring 0.4 m in length with a temperature-controlled reservoir containing solid alkali salt. The cell was placed in a furnace and the alkali vapours generated from the reservoir have direct access to the measuring chamber. Investigations of potassium chloride (KCl) were made on sublimated vapour at temperatures 650, 700, 750, 780, and 800 °C while the reservoir temperature was kept 50 °C lower to avoid condensation. The cell provides stable KCl vapour pressures, and the furnace provides a homogenous temperature profile along the cell. KCl vapour pressures are well characterised and conform the base for determination of the KCl concentration in the cell. The alkali chloride levels matched the concentration range of the absorption setup and indicated a previously employed calibration method to overestimate KCl concentrations. The KCl absorption cross sections for wavelengths λ =197.6 nm and λ =246.2 nm were calculated to be 3.4 × 10-17 and 2.9 × 10-17 cm2/molecule, respectively. The absorption cross section spectra did not show any structural differences with increasing temperature, which could indicate influence of dimers or significant changes of the population in the KCl vibrational states. The KCl absorption cross sections thus did not show any temperature dependence in the temperature region of 700-800 °C. Moreover, the applicability of the calibration cell for measurement of other alkali chlorides and hydroxides is discussed.

  10. Determination of iodine via the spectrum of barium mono-iodide using high-resolution continuum source molecular absorption spectrometry in a graphite furnace

    NASA Astrophysics Data System (ADS)

    Huang, Mao Dong; Becker-Ross, Helmut; Florek, Stefan; Okruss, Michael; Welz, Bernhard; Morés, Silvane

    2009-07-01

    Molecular absorption spectra of the diatomic molecules AlI, GaI, InI, TlI, MgI, CaI, SrI and BaI, generated in a graphite furnace, were studied using a high-resolution echelle spectrometer with the aim of finding a simple, reliable and sensitive analytical method for the determination of iodine. Among them, the barium mono-iodide (BaI) was found to have the strongest absorption bands around 538 nm and 560 nm, each of them consisting of a series of well-resolved rotational lines with half-widths of about 40-50 pm. The strongest BaI line, the band head at 538.308 nm has been evaluated systematically for its analytical use for the determination of iodine. High concentrations of hydrochloric acid (or chloride), hydrofluoric acid (or fluoride), iron, potassium and sodium resulted in significant reduction of the BaI molecular absorption. Apart from this, no other serious spectral or non-spectral interference has been observed. Different chemical forms of iodine, such as iodide, iodate and organically bound iodine produced identical BaI absorption sensitivity. The detection limit for iodine was 600 pg, and the calibration curve was linear up to 250 ng iodine. Two real samples with different chemical forms of iodine were analyzed using the proposed method. One sample was an iodide pill with a specified iodide content of 200 mg, the other one was a thyroid hormone pill with a specified content of 63.5 mg. The results were in good or satisfactory agreement with those of independent methods, the potentiometric titration and the inductively coupled plasma time-of-flight mass spectrometry (ICP-ToF-MS); the deviations were 2% and 8% for the iodide and the thyroid hormone sample, respectively. The relative standard deviation of the analytical results ( n = 3) was below 2%.

  11. Measurement of temperature profiles in flames by emission-absorption spectroscopy

    NASA Technical Reports Server (NTRS)

    Simmons, F. S.; Arnold, C. B.; Lindquist, G. H.

    1972-01-01

    An investigation was conducted to explore the use of infrared and ultraviolet emission-absorption spectroscopy for determination of temperature profiles in flames. Spectral radiances and absorptances were measured in the 2.7-micron H2O band and the 3064-A OH band in H2/O2 flames for several temperature profiles which were directly measured by a sodium line-reversal technique. The temperature profiles, determined by inversion of the infrared and ultraviolet spectra, showed an average disagreement with line-reversal measurements of 50 K for the infrared and 200 K for the ultraviolet at a temperature of 2600 K. The reasons for these discrepancies are discussed in some detail.

  12. Differential absorption lidar technique for measurement of the atmospheric pressure profile

    NASA Technical Reports Server (NTRS)

    Korb, C. L.; Weng, C. Y.

    1983-01-01

    A new two-wavelength lidar technique for remotely measuring the pressure profile using the trough absorption region between two strong lines in the oxygen A band is described. The theory of integrated vertical path, differential ranging, and horizontal-path pressure measurements is given, with methods to desensitize and correct for temperature effects. The properties of absorption troughs are described and shown to reduce errors due to laser frequency jitter by up to two orders of magnitude. A general analysis, including laser bandwidth effects, demonstrates that pressure measurements with an integrated-vertical-path technique are typically fifty times more accurate than with a differential ranging technique. Simulations show 0.1-0.3 percent accuracy for ground and Shuttle-based pressure-profile and surface-pressure experiments.

  13. Highly sensitive absorption measurements in lithium niobate using whispering gallery resonators

    NASA Astrophysics Data System (ADS)

    Leidinger, Markus; Buse, Karsten; Breunig, Ingo

    2015-02-01

    The absorption coefficient of undoped, congruently grown lithium niobate (LiNbO3) for ordinarily and extraordinarily polarized light is measured in the wavelength range from 390 to 2600 nm using whispering gallery resonators (WGRs). These monolithic cavities guide light by total internal reflection. Their high Q-factor provides several hundred meters of propagation for the coupled light in millimetre size resonators allowing for the measurement of absorption coefficients below 10-2 cm-1, where standard methods such as Fourier-transform or grating spectroscopy meet their limit. In this work the lowest measured value is 10-4 cm-1 at 1700 nm wavelength. Furthermore, the known OH- overtone at 1470 nm wavelength can be resolved clearly.

  14. Resonant tube for measurement of sound absorption in gases at low frequency/pressure ratios

    NASA Technical Reports Server (NTRS)

    Zuckerwar, A. J.; Griffin, W. A.

    1980-01-01

    The paper describes a resonant tube for measuring sound absorption in gases, with specific emphasis on the vibrational relaxation peak of N2, over a range of frequency/pressure ratios from 0.1 to 2500 Hz/atm. The experimental background losses measured in argon agree with the theoretical wall losses except at few isolated frequencies. Rigid cavity terminations, external excitation, and a differential technique of background evaluation were used to minimize spurious contributions to the background losses. Room temperature measurements of sound absorption in binary mixtures of N2-CO2 in which both components are excitable resulted in the maximum frequency/pressure ratio in Hz/atm of 0.063 + 123m for the N2 vibrational relaxation peak, where m is mole percent of added CO2; the maximum ratio for the CO2 peak was 34,500 268m where m is mole percent of added N2.

  15. Ultraviolet-absorption photometer for measurement of ozone on a rocket-boosted payload

    NASA Astrophysics Data System (ADS)

    Sen, B.; Sheldon, W. R.; Benbrook, J. R.

    1996-10-01

    We developed a rocket payload to perform in situ measurements of atmospheric ozone at the University of Houston. The ozone detector is a dual-beam UV-absorption photometer that uses the 253.7-nm radiation from a low-pressure mercury-vapor lamp to illuminate two identical absorption chambers. We describe the design features and the operation of the instrument. The fundamental resolution of the photometer is shown to be 2.7 10 15 molecules m 3 . We present the ozone profile measured during parachute descent following boosted ascent to 60 km by a Nike Orion rocket. The uncertainty in the measurement of this ozone profile is estimated to be 8.2 .

  16. Results of measurement of radio wave absorption in the ionosphere by the AI method

    NASA Technical Reports Server (NTRS)

    Korinevskaya, N. A.

    1972-01-01

    Median noon absorption values for each month from 1964 through 1967, the diurnal variations of absorption on the regular world days, and the seasonal variations of absorption are given. The dependence of the absorption coefficient on sunspot number is analyzed.

  17. Aerosol absorption measurement at SWIR with water vapor interference using a differential photoacoustic spectrometer.

    PubMed

    Zhu, Wenyue; Liu, Qiang; Wu, Yi

    2015-09-07

    Atmospheric aerosol plays an important role in atmospheric radiation balance through absorbing and scattering the solar radiation, which changes local weather and global climate. Accurate measurement is highly requested to estimate the radiative effects and climate effects of atmospheric aerosol. Photoacoustic spectroscopy (PAS) technique, which observes the aerosols on their natural suspended state and is insensitive to light scattering, is commonly recognized as one of the best candidates to measure the optical absorption coefficient (OAC) of aerosols. In the present work, a method of measuring aerosol OAC at the wavelength where could also be absorbed by water vapor was proposed and corresponding measurements of the absorption properties of the atmospheric aerosol at the short wave infrared (SWIR, 1342 nm) wavelength were carried out. The spectrometer was made up of two high performance homemade photoacoustic cells. To improve the sensitivity, several methods were presented to control the noise derived from gas flow and vibration from the sampling pump. Calibration of the OAC and properties of the system were also studied in detail. Using the established PAS instrument, measurement of the optical absorption properties of the atmospheric aerosol were carried out in laboratory and field environment.

  18. Measurement of acetaldehyde in exhaled breath using a laser absorption spectrometer

    NASA Astrophysics Data System (ADS)

    Kamat, Pratyuma C.; Roller, Chad B.; Namjou, Khosrow; Jeffers, James D.; Faramarzalian, Ali;